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Publication numberUS3652317 A
Publication typeGrant
Publication dateMar 28, 1972
Filing dateMay 1, 1970
Priority dateMay 1, 1970
Publication numberUS 3652317 A, US 3652317A, US-A-3652317, US3652317 A, US3652317A
InventorsPaolo Della Porta, Tiziano A Giorgi, Bruno Kindl, Mario Zucchinelii
Original AssigneeGetters Spa
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Method of producing substrate having a particulate metallic coating
US 3652317 A
Abstract
A method of producing a substrate having a particulate coating of high surface area to mass ratio, said method comprising in sequence the steps of:
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Description  (OCR text may contain errors)

Unite ttes Ptent llllelllla Port/a et a1. Mar. 2%, 19972 541 MEETHtJ D @1 1 PRQD UCING SUBSTRATE 3,549,357 12/1970 Osborne ..117/31 x MAW/ENG A IPARFHCUH'ATE METALLHQ FOREIGN PATENTS OR APPLICATIONS @UATENG 5,774 12/1915 Great Britain ..117/31 1721 P911110 61W; 198 085 6/1967 0.5.5.12. ..117/31 11111-111110 lflndl; Marlo Zucclhlnelll, all of M1131" [my Primary Examiner-John F. Campbell [73] Assignee: SAJES. Getter-s S. p.A., Milan, Italy Assistant Examiner D0flald 3 3 Att0mey-Burns, Doane, Benedict, Swecker and Mathis [22] Filed: May 11, 1970 211 Appl. No.: 33,794 [57] ABSTRACT A method of producing a substrate having a particulate coat- W A P WWRPM ing of high surface area to mass ratio, said method comprising [63] Continuation-impart of Ser. No. 527,906, Feb. 16, in Sequence the Steps of:

1966, abandoned.

I. disposing particles between a substrate and an inter- [52] US. (11.. ..117/22, 117/31, 117/130 R, mediate body wherein the particles are harder than th 3 117/160 29/1912 29/420 29/423, 29/527-7 substrate; and the intermediate body is softer than the r zg/DIG- 264/111 252/181-7 particles but is harder than the substrate: [51;] 1113111. C11 ..B'Il5b 7/l, B44c 1/06, 1344C 1/08 [L compressing the Substrate and intermediate body with [51 lFnelld ntfieareh ..29/191.2,420, 423, 527.7, particles therebetween whereby the intermediate body 29/D1G. 32; 264/111; 117/100 M, 31, 130 R, 22, ushes the particles into the substrate; and

160 R; 252/181] [11. removing the intermediate body from the particles leaving them embedded in the substrate. [56] lReEerences Cited UNITED STATES PATENTS The coating substrates produced by the process of the present invention find utility as catalytic devices to accelerate or re- 2,373,405 4/1945 Lowlt ..29/420 tat-d Chemical reactions as getter devices to Sorb residual 2-626458 1/1953 gases in closed vessels such as electronic tubes, and with 3,002,834- 10/1961 D1 Pasquale ..29/420 UX f th processing as capacitors 3,093,501 6/1963 Clayton ..117/31 X 3,152,892 10/1964 Clark ..29/420 UX 16 Claims, 4 Drawing Figures PATENTEU MAR 2 8 I972 lNVENToRs PAOLO dELLA PORTA TIZIANO A. GIORGI BRUNO KINDL MARIO ZUCCHINELLI PATENTEDmza 1972 3.652.317

sum 2 or 2 2-i- 2O B IFFI IP QQM L 'IIIIII l FIG.4

INVENTORS PAOLO dELLA PORTA TIZIANO A- GIORGI BRUNO KINDL MARIO ZUCCHINELLI Mlli'lilillfillill @IF FERGIDIUCIING SUBSTRATE HAVWG A FAIRTHUJLATE METALLIIC COATING CROSS rdEFERENCE TO RELATED APPLICATIONS This application is a continuation-in-part of US. application Ser. No. 527,906 filed Feb. 16, 1966, now abandoned, the disclosure of which is incorporated herein by reference.

Processes for producing substrates having thereon a particulate metallic coating are notoriously well known in the art. However, most prior processes require the use of a binder to hold the metal particles to the substrate. In an effort to avoid the use of a binder it has been suggested to place the metal particles on the substrate to be coated and then pass these between the nip or rotating rolls to embed the particles in the surface of the substrate. However, such processes suffer from a number of disadvantages. One disadvantage is the wear of the rolls which is especially acute when the metal particles are hard. This wear of the rolls necessitates their frequent replacement with a concurrent expense. However, an even more troublesome effect of the wear of the rolls is their inability to exert an even pressure on the particles with the result that only portion of the substrate is coated or alternatively an uneven coating results. Another disadvantage of the use of rolls in contact with metal particles is that the action of the rolls on the particles substantially reduces their total surface area. This especially troublesome when the desired coated substrate is one preferably having a high surface area to mass ratio of the coating particles.

lvlarly of the prior processes require the use of superambient temperatures increasing expense and the necessity for elaborate controls. Many other prior processes do not produce a coated substrate having physical characteristics rendering it suitable for the intended use. Examples of such physical characteristics include among others a high heat transfer coefficient between the metal particles and the substrate, a resistance of the coated substrate to mechanical shocks, to ultrasonic vibrations, and to thermally induced stresses such as are caused by heating the coated substrate to high temperatures such as those of 1,000 C. and higher. Many of these coated substrates lack freedom from loose particles which may be created by separation ofparticles of the metallic coating from the substrate.

Because of the above described disadvantages such processes have been found unsuitable for the production of getter devices, catalytic devices, and capacitors.

it is therefore an object of the present invention to provide an improved method for producing a substrate having a particulate metallic coating thereon which method is substantially free of one or more of the disadvantages ofprior methods.

Another object is to provide an improved method which does not require the use ofa binder.

a further object is to provide an improved method which can be practiced at ambient temperatures.

A still further object is to provide an improved method employing roll which are not subject to wear.

i another object is to provide an improved method for producing a coated substrate such as those suitable to be used a catalytic devices, getter devices, or capacitors.

"till another object is to provide an improved method for producing a coated substrate which has the above described desirable physical characteristics.

Still another object is to provide a method for producing an improved getter device having a high surface area to mass ratio the getter metal and which is free of loose particles.

A tiitional objects and advantages of the present invention wili be apparent to those skilled in the art by reference to the detailed description thereof and drawings wherein: itt t is a cross-sectional view with an enlargement of about 300 diameters of a coated substrate produced by the method of the present invention wherein the coating has a thickness approximately equal to one particle diameter and;

lFlG. is a cross-sectional view with an enlargement of about 300 diameters of a coated substrate produced by the method of the present invention wherein the particulate metallic coating has a thickness of approximately 3 particle diameters, this figure being a drawing corresponding to a microphotograph representing the structure taken along line 2-2 of FIG. d and;

FIG. 3 is a cross-sectional view with an enlargement of about 1,300 diameters of a coated substrate produced by the method of the present invention wherein the original substrate comprised a hard base having a softer metallic coating thereon and;

FIG. 4 is a schematic representation of an apparatus suitable for practicing the method of the present invention.

In accordance with the present invention there is provided a method of producing a substrate having a particulate metallic coating of high surface area to mass ratio and usually greater than 2 cm."'/mg. The method comprises in sequence the steps of: r

I. disposing metal particles between a substrate and an intermediate body wherein the particles are harder than the substrate; and the intermediate body is softer than the particles but is harder than the substrate;

II. compressing the substrate an intermediate body, with particles therebetween whereby the intermediate body pushes the particles into the substrate; and

III. removing the intermediate body from the particles leaving them embedded in the substrate.

Referring now to the drawings and in particular to FIG. ll there is shown a substrate 1 of stainless steel having an upper coating 2 and a lower coating 3 comprising metal particles of a zirconium alloy partially embedded in the surface of the substrate 1. FIG. 2 shows an iron substrate i having coatings 5 and 6 wherein these coatings 5 and 6 have a total thickness which is approximately equal to three times the diameter of a single particle. As can be seen the metal particles in contact with the substrate 4 are partially embedded therein whereas the other particles are attached to one another or held in place by small cold microwelds (not shown) between the individual particles. FIG. 3 discloses a base 7 of iron having aluminum thereon which actually forms the substrate 8. The particles forming the coating 9 are partially embedded in this substrate 8.

Referring now to FIG. 4 there is shown an apparatus it) suitable for practicing the process of the present invention. in the practice of this process loose metal particles ii and R2 are disposed respectively between a substrate 13 and an upper intermediate body 14 and the substrate 13 and a lower intermediate body 15. Most conveniently the metal particles ii are placed on the substrate 13 whereas the metal particles M are placed on the lower intermediate body 15 to form a composite structure which is passed between the nip of two rolls i6 and 17 rotating respectively in the direction of arrows l8 and 19. The apparatus 10 is provided with means for maintaining the distance between the rolls less than the combined thickness of the substrate 13, particles Ill and 17., and intermediate bodies 14 and I5. In the preferred embodiment wherein the intermediate bodies 14 and 15 are work-hardenable the rolls id and 17 press the intermediate bodies lid and 15 with a force such that the intermediate bodies M and 15 undergo plastic deformation with concurrent work-hardening while effectively pushing the metal particles ii and 112 into the substrate 33 without substantially reducing the total surface area of the metal particles ill and 12.

The entire composite structure then leaves the nip between rolls i6 and 17 with the intermediate bodies M and i5 adlrering to the metal particles Ill and 12 which are embedded in the substrate 13 and are welded to one another by cold microwelds. The intermediate bodies l4 and E5 are then removed leaving behind the coated substrate 26]. By virtue of the above described relationship in hardness between the metal particles 11 and 12, the substrate l3 and the intermediate bodies Ml and 15 the metal particles 11 and i2 adhere substantially completely to the substrate 13 rather than to the intermediate bodies M and 15. This relationship in hardness is critical to the successful practice of the method of the present invention. For example, if the intermediate bodies 14 and 115 are of the same hardness as the substrate R3 the particles ll and i2 will be randomly embedded in the substrate 113 and the intermediate bodies lid and 115. On the other hand if the substrate if) is harder than the intermediate bodies l4 and 15 the particles will preferentially embed themselves into the intermediate bodies M and iii. if the particles ii and 12 are softer than either the intermediate bodies 114 and 15 or the substrate i3 they will be plastically deformed losing their surface area and will not become embedded in the substrate 113.

The metal particles can be of widely varying particle sizes but are generally those which pass through a US. standard screen of 10 mesh per inch and are preferably those which pass through a US. standard screen of 100 mesh per inch and are retained on a screen of 600 mesh per inch.

Broad and preferred ranges of Vickers hardness for the intermediate body, the metallic particles and the substrate are given in the following table:

Vickers Hardness Component Broad Preferred Example Range Range (kg/mm) g/mm) (kg/mm) intermediate body l-60O 10il-300 180 Particles l00=c 200-800 400 Substrate l-400 10-200 90 The values given in this table are non-limiting in the sense that specific values within the above ranges must be chosen while maintaining the herein-described hardness relationship. in a preferred embodiment of the present invention the intermediate body has a Vickers hardness at least 50 and preferably at least 100 kgjmm. less than the particles; and the substrate has a Vickers hardness of at least lll and preferably at least ill) kgJmm. less than the intermediate body.

The particles of the metal to be embedded in the substrate are chosen with respect to the desired end use of the product. Thus if a getter device is desired particles of a non-evaporable getter metal are employed whereas if a catalytic device is desired particles of a catalyst metal are chosen. Finally if a capacitor is desired metallic particles are employed which are electrically conductive in the broadest aspect any prior known non-evaporable getter metal can be employed in the production of getter devices. Examples of suitable getter metals include among others zirconium, titanium, tantalum, niobium, vanadium mixtures thereof and alloys thereof with one another and with other metals which do not materially reduce the gas sorptive capacity of these getter metals. The preferre getter metal is an alloy of to 30 and preferably 13 to 13 weight percent aluminum balance Zirconium. When it is desired to produce catalytic devices the metal particles are those which have heretofore been found to catalyze the particular chemical reaction. Examples of suitable catalytic rials include among others platinum, zirconium, vanadium, tantalum. Examples of electrically conductive particles suitable for producing capacitors include among others iron, silver, copper and preferably aluminum.

The substrate and the intermediate bodies can be of any metal which has the herein described hardness relationship. Examples of suitable metals include among others soft iron, steel, and stainless steel. it must be emphasized that the chemical nature of the elements making up the alloys emplayed as substrates and intermediate bodies is not critical. in fact it is conceivable that alloys of identical chemical composition can be employed as both provided that they have differing hadnesses. As is apparent to those skilled in the art differing resses can be imparted by conventional metallurgical techniques such as heat treatment, cold rolling and the like.

The invention is further illustrated by the following examples in which all parts and percentages are by weight unless otherwise indicated. These non-limiting examples are illustrative of certain embodiments designed to teach those skilled in the art how to practice the invention and to represent the best mode contemplated for carrying out the invention.

XAMPLE 1 This example illustrates the method of the present invention wherein the resulting structure is a getter device.

Referring to H6. 4 finely divided particles of a nonevaporable getter alloy available from SAES Setters S.p.A. as St llllll is placed on an iron substrate 0.0M) inches thick. The St 101 is an alloy of 16 percent aluminum, balance zirconium and passes through a screen of mesh per inch and is retained on a screen of 600 mesh per inch. The particles of St 101 in their sheet form exhibit a Vickers hardness of 400 kg./mm. The substrate has a Vickers hardness of 90 kg./mm. A single intermediate body of iron having a Vickers hardness of 180 kg./mm. and a thickness of 0.010 inches is placed on top of the metal particles and the resultant composite passed between the nip of two rotating rolls. The intermediate body is then removed leaving the particles embedded in the substrate.

XAMPLE 2 This example illustrates the process of the present invention wherein the resultant product is a catalytic device.

The procedure of Example l is repeated except that the particles of St 101 are replaced with platinum and the substrate is replaced with one of aluminum having a Vickers hardness of 50 kg/mm. and the intermediate body is replaced by one of iron having a Vickers hardness of kg./mm. The resultant.

catalytic device functions satisfactorily to increase the reaction rate of a chemical reaction.

Although the invention has been described in considerable detail with reference to certain preferred embodiments thereof, it will be understood that variations and modifications can be effected within the spirit and scope of the invention as described above and as defined in the appended claims.

We claim:

ll. A mechanical method of producing a metallic substrate having a metallic particulate coating of high surface area to mass ratio, said method comprising in sequence the steps of:

l. disposing metallic particles between the metallic substrate and an intermediate body wherein the particles are harder than the substrate; and the intermediate body is softer than the particles but is harder than the substrate;

ll. employing a compressing means in order to compress the substrate and intermediate body, with particles therebetween whereby the intermediate body pushes the particles into the substrate; and

ill. removing the intermediate body from the particles leaving them embedded in the substrate.

2. The process of claim ll wherein the particles are placed on the substrate, and wherein an additional amount of particles are placed on a second intermediate body which is on the side of the substrate opposite the first intermediate body in order to produce a structure having particles embedded on both sides of the substrate.

3. The process of claim ll wherein the particles are susceptible to cold welding to one another and to the substrate.

The process of claim 1 wherein the particles are of a size such that they pass through a US. standard screen of 10 mesh per inch.

5. The process of claim l wherein the substrate has a Vickers hardness of 10 to 200 kg./mm.

6. The process of claim 11 wherein the intermediate body has a Vickers hardness of l00 to 300 kgJmmF.

7. The process of claim l wherein the metallic particles have a Vickers hardness of 200 to 800 lrg/mmf.

ii. The process of claim it wherein the intermediate body has a Vickers hardness at least 50 kg./mrn. less than the particles.

9. The process of claim it wherein the substrate has a Vickers hardness at least 40 kg./mrn. less than the intermediate body.

lib. A mechanical method of producing a structure of high area having particles of metal embedded in a metallic substrate, said method comprising in sequence the steps of:

l. disposing loose particles of metal between the metallic substrate and a work hardenable intermediate body wherein the particles are harder than the substrate; and the intermediate body is softer than the particles but is harder than the substrate;

passing the substrate and intermediate body, with loose particles therebetween, between the nip of two rotating rolls wherein the distance between the rolls in less than the combined thickness of the substrate the intermediate body and the mass of loose particles; whereby the intermediate body undergoes plastic deformation with the concurrent work hardening while effectively pushing the particles into the substrate without substantially reducing V the total surface area of the particles; and V V, V, 7

ill. removing the intermediate body from the particles leaving them partially embedded in the substrate.

The process of claim ll wherein the distance between the surnames of the rolls is suiiiciently small that the intermediate body and the substrate both exhibit plastic deformation, but is not so small as to substantially reduce the total surface area of the particulate material.

A mechanical method of producing a getter device having r articles of a non-evaporable getter metal embedded in a me allic substrate, said method comprising in sequence the step oi":

disposing particles of a non-evaporable getter metal between the metallic substrate and an intermediate body wherein the particles are harder than the substrate and the intermediate body is softer than the particles but is harder than the substrate;

ll. passing the substrate and intermediate body, with particles therebetween, between the nip of two rotating rolls whereby the intermediate body pushes the particles into the substrate; and

ill. removing the intermediate body from the particles leaving them embedded in the substrate.

113. The process of claim 12 wherein the non-evaporable getter material is a zirconium-aluminum alloy.

The process of claim i3 wherein the zirconium-aluminum alloy contains to 30 weight percent aluminum balance zirconium.

15. A mechanical method of producing a getter device having particles of a non-evaporable getter metal embedded in a metallic substrate, said method comprising in sequence the steps of:

l. disposing loose particles of a non-evaporable getter metal between the metallic substrate and an intermediate body wherein the particles are harder than the substrate and the intermediate body is softer than the particles but is harder than the substrate and is in a work-hardenable condition;

ll. passing the substrate and intermediate body, with loose particles therebetween, between the nip of two rotating rolls wherein the distance between the rolls is less than the thickness of the substrate and intermediate body with loose particles therebetween; whereby the intermediate body undergoes plastic deformation with concurrent work hardening while effectively pushing the particles into the substrate without substantially reducing their surface area; and

Ill. removing the intermediate body from the particles leaving them partially embedded in the substrate.

16. A mechanical method of producing a getter device having particles of a non-evaporable getter metal embedded in a metallic substrate, said method comprising in sequence the steps of:

l. disposing loose particles of a non-evaporable getter metal consisting essentially of an alloy of 13 to 18 weight percent aluminum balance zirconium between the substrate and a work hardenable intermediate body wherein the intermediate body has a Vrckers hardness at least 100 kgjmm. less than the particles and the metallic substrate has a Vickers hardness at least kg/mm less than the intermediate body;

ll. passing the substrate and intermediate body, with loose particles therebetween, between the nip of two rotating rolls wherein the distance between the rolls is less than the thickness of the substrate and intermediate body with loose particles therebetween; whereby the intermediate body undergoes plastic deformation with concurrent work hardening while effectively pushing the particles into the substrate without substantially reducing their surfaces arca; and

Ill. removing the intermediate body from the particles leaving them partially embedded in the substrate.

*srerrn

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Classifications
U.S. Classification427/194, 428/557, 428/614, 427/198, 419/66, 428/653, 502/527.24, 419/69, 252/181.7, 29/DIG.320, 428/555, 427/81, 427/123, 29/527.7, 29/423
International ClassificationC23C24/02
Cooperative ClassificationY10S29/032, C23C24/02
European ClassificationC23C24/02