IP Library Granted Patent US 9,447,493
Granted Patent B2
US 9,447,493 · App. 13/579,862 · Granted Sep 20, 2016

Plasma sputtering process for producing particles

Inventors: Ulf Helmersson (Brokind, SE); Nils Brenning (Johanneshov, SE); Daniel Soderstrom (Boxholm, SE)
Assignee: Plasmadvance AB
C23C14/223B22F9/12C23C14/3485C23C14/54C23C14/544H01J37/34B22F2999/00
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Quick Facts
Patent No.
US 9,447,493
App. No.
13/579,862
Granted
Sep 20, 2016
Kind
B2
Abstract

A high production rate plasma sputtering process for producing particles having a size of 10 μm or less is disclosed. The process causes ionization of at least a part of the sputtered target atoms and is performed at such parameters that the pick-up probability of ionized sputtered target atoms on the surface of grains is high.

Claims (71)

1. A plasma sputtering process for producing particles having a size of about 1 nm to about 10 μm by growth to said size of the particles through pick-up of sputtered target atoms on the surface of grains, the grains constituting previously formed particles or particle nuclei, the process comprising

providing a target in a plasma generating apparatus, said apparatus having a characteristic length L c wherein L c 3 equals the volume of the plasma generated in said apparatus,

introducing a process gas into said plasma generating apparatus and controlling the pressure inside the plasma generating apparatus in order to obtain a process gas number density n G ,

creating a plasma inside said plasma generating apparatus and controlling the energy provided to said plasma in order to obtain a plasma electron number density n e and a plasma electron temperature T e ,

sputtering atoms from said target by means of said plasma,

allowing the sputtered atoms to be picked-up on the surface of the grains, the grains being present in the plasma, thus producing the particles having a size of about 1 nm to about 10 μm, and

collecting the produced particles,

wherein the plasma electron number density n e and plasma electron temperature T e are sufficient to cause ionization of at least a part of the sputtered target atoms thus resulting in a pick-up flux of ionized sputtered target atoms on the surface of the grains;

wherein the following criterion is fulfilled L ITA /L c ≦0.5

where L ITA is the mean free path of the ionized sputtered target atoms inside said plasma,

wherein the plasma generating apparatus is operated by a pulsed electric power supply with a frequency of at least 100 Hz and with a duration of the pulses of at least 5 microseconds, and

wherein the energy provided to the plasma is sufficient to obtain ionization of at least 20 % of the sputtered atoms in said plasma.

2. The process of claim 1 wherein Γ ITA /(Γ ITA +Γ NTA ) 0.5, wherein Γ ITA is the pick-up flux of ionized target atoms on the surface of grains and Γ NTA is the pick-up flux of neutral target atoms on the surface of grains.

3. The process of claim 1 wherein the energy provided to the plasma is sufficient to obtain ionization of at least 30% of the sputtered atoms in said plasma.

4. The process of claim 1 wherein the plasma generating apparatus is a hollow cathode apparatus.

5. The process of claim 1 wherein the plasma generating apparatus is a magnetron sputtering apparatus.

6. The process of claim 1 wherein (1+3L c /L ITA )(1+4W e /W ITA )>10, wherein W ITA is the average kinetic energy of ionized sputtered atoms in said plasma and W e is the average electron kinetic energy inside said plasma related to T e through W e =(3/2)k B T e .

7. The process of claim 1 wherein the electric power is supplied essentially in the form of square pulses.

8. The process of claim 1 wherein the pulsed electric power supply is applied with a frequency of 200 -2000 Hz and with a duration of the pulses of 10-100 microseconds.

9. The process of claim 1 wherein the average power applied to the cathode is at least 30,000 W/m 2 .

10. The process of claim 1 wherein the process gas number density n G and the electron number density n e are such that

W

ITA

W

e

0.5

wherein W ITA is the average kinetic energy of ionized sputtered atoms in said plasma and W e is the average electron kinetic energy inside said plasma related to T e through W e =(3/2)k B T e .

11. The process of claim 1 wherein

L

ITA

L

c

0.4

.

12. The process of claim 11 wherein

W

ITA

W

e

0.4

.

13. The process of claim 1 wherein the process gas is an inert gas, a reactive gas, a gas mixture of inert gases, or a gas mixture comprising at least a reactive gas.

14. The process of claim 1 wherein said plasma is created at least partly of said process gas.

15. The process of claim 1 wherein the process gas is an inert gas, and the process further comprises introducing a reactive gas or a gas mixture comprising a reactive gas, into said plasma generating apparatus.

16. The process of claim 1 wherein said grains are introduced into said plasma generating apparatus.

17. The process of claim 1 wherein said grains are formed in-situ in said plasma generating apparatus.

18. The process of claim 1 wherein the plasma electron number density n e is at least 10 17 per m 3 .

19. The process of claim 1 wherein the process produces particles having a size ranging from about 5 nm to about 500 nm.

20. The process of claim 2 wherein Γ ITA /(Γ ITA +Γ NTA ) ≧0.66.

21. The process of claim 20 wherein Γ ITA /(Γ ITA +Γ NTA ) ≧0.70.

22. The process of claim 11 wherein

L

ITA

L

c

0.3

.

23. The process of claim 12 wherein

W

ITA

W

e

0.3

.

24. The process according to claim 1 , wherein collecting the produced particles comprises cooling the produced particles and thereafter collecting the particles on a substrate.

25. The process according to claim 1 , wherein collecting the produced particles is performed by a system wherein the produced particles are suspended in a carrier gas.

Assignments (6)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 8, 2019
From: PLASMADVANCE AB
To: IONAUTICS AB
Reel/Frame 049113/0125 →
CORRECTIVE ASSIGNMENT TO CORRECT THE SPELLING OF THE STREET ADDRESS FOR BOTH THE ASSIGNOR AND ASSIGNEE PREVIOUSLY RECORDED ON REEL 038479 FRAME 0164. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded May 13, 2016
From: TIÅ AB
To: PLASMADVANCE AB
Reel/Frame 038745/0914 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 5, 2016
From: TIÅ AB
To: PLASMADVANCE AB
Reel/Frame 038479/0164 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 17, 2012
From: HELMERSSON, ULF; BRENNING, NILS; SODERSTROM, DANIEL
To: PLASMADVANCE AB
Reel/Frame 028807/0817 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 17, 2012
From: PLASMADVANCE AB
To: DELPHINARIUM 221 AB
Reel/Frame 028807/0975 →
CHANGE OF NAME Recorded Aug 17, 2012
From: DELPHINARIUM 221 AB
To: TIA AB
Reel/Frame 028808/0083 →
Priority Claims (1)
SE 1050173 · Feb 24, 2010 · national
Continuity (2)
Provisional Application 61307475 · Feb 24, 2010
Related Publication 20120305385A1 · Dec 6, 2012