Electrohydrodynamic spraying to produce ultrafine particles

• US 4,264,641 A
• Filed: 05/10/1978
• Issued: 04/28/1981
• Est. Priority Date: 03/17/1977
• Status: Expired due to Term

• Current Assignee: Phrasor Technology Incorporated
• Original Assignee: Phrasor Technology Incorporated
• Inventors: Mahoney, John F., Perel, Julius, Vickers, Kenneth E.
• Primary Examiner(s): Beck, Shrive P.
• Application Number:
  US05/904,580
• Time in Patent Office: 1,084 Days
• Field of Search: 427/13, 427/30, 427/422, 264/10, 264/12, 75/0.5 C, 425/6, 361/228
• US Class Current: 427/483
• CPC Class Codes: B05B 5/001 incorporating means for heating or cooling, e.g. the material to be sprayed
• CPC Class Codes: B05B 5/025 Discharge apparatus, e.g. electrostatic spray guns
• CPC Class Codes: B05B 5/0255 spraying and depositing by electrostatic forces only
• CPC Class Codes: B05B 9/002 incorporating means for heating or cooling, e.g. the material to be sprayed
• CPC Class Codes: B22F 2998/00 Supplementary information concerning processes or compositions relating to powder metallurgy
• CPC Class Codes: B22F 3/115 by spraying molten metal, i.e. spray sintering, spray casting
• CPC Class Codes: B22F 9/14 using electric discharge
• CPC Class Codes: C23C 4/137 Spraying in vacuum or in an inert atmosphere

Abstract

Amorphous or microcrystalline alloy powder is prepared by the rapid quenching of ultrafine metallic spheroids generated from the molten metal state. The molten metal droplets are formed when an intense electric field (10⁵ V/cm) is applied to the surface of liquid metal held in a suitable container. The interactions between the intense electric field and liquid surface tension disrupts the metal surface, resulting in a beam of positively charged droplets. The liquid metal spheres generated by this electrohydrodynamic process are subsequently cooled by radiative heat transfer. Rapid cooling of the droplets may be accomplished by heat transfer to a low pressure gas by free molecular heat conductivity. Quenching rates exceeding 10⁶ °K./sec are possible using this technique. Thin film coatings are prepared by electrohydrodynamically spraying a beam of charged droplets against a target (substrate). The target can be electrically controlled to effect the charged particles impact. The materials to be sprayed electrodynamically can be varied in both throughput and species such that a target can have multimaterial layers being deposited coincidentally or sequentially. The ultra small droplet size will enhance the physical properties by reducing skin stresses and enhance the optical properties by reducing the growth of crystallites in the film. Precise layers can be deposited from extremely thin films to thick filters for optical characteristics into the infrared. All materials that can be molten and contained can be electrohydrodynamically sprayed and controlled for depositions upon a substrate material.

Claims

1. A method of forming high melting temperature metal alloys in the form of ultrafine particles ranging in size from sub-micron to about 100 microns by electrohydrodynamic spraying which comprises:

liquefying the metal alloy;

pneumatically feeding the molten metal alloy to a capillary nozzle to form a liquid meniscus at the tip of the nozzle;

applying a positive electric field to the molten metal alloy to create electrostatic forces which are high enough to overcome the surface tension of the liquid meniscus to thereby generate a beam of positively charged ultrafine droplets of said metal alloy;

solidifying the ultrafine droplets; and

collecting the resulting ultrafine metal alloy particles.

2. The method of claim 1 which is carried out in a vacuum chamber evacuated to at most about 0.5 atmospheres.

3. The method of claim 2 wherein said vacuum is about 10^-5 to about 10^-6 torr.

4. The method of claim 1 wherein said droplets range in size from about 0.01 microns to about 1 micron.

5. The method of claim 1 wherein the droplets of said molten metal alloy are collected in the form of a thin film coating by impinging the droplets on a target substrate before said droplets completely solidify.

6. The method of claim 5 wherein said target substrate is positively charged to cause said positively charged droplets to decelerate before impinging on said target.

7. The method of claim 5 wherein said target substrate is non-conductive and wherein when said positively charged droplets impinge on said substrate the resulting buildup of charge generates a floating positive potential at the substrate surface to thereby decelerate the remaining positively charged droplets.

8. The method of claim 1 wherein said metal alloy has a melting temperature of over 500°

C.

9. The method of claim 1 wherein said metal alloy is an iron, nickel or copper alloy having a melting temperature of at least 1000°

C. and is non-wetting with respect to the capillary nozzle material.