Chemical-mechanical planarization slurries and powders and methods for using same

• US 6,730,245 B2
• Filed: 01/02/2001
• Issued: 05/04/2004
• Est. Priority Date: 02/24/1997
• Status: Expired due to Fees

• Current Assignee: Cabot Corporation
• Original Assignee: Superior Micropowders
• Inventors: Hampden-Smith, Mark J., Caruso, James, Kodas, Toivo T., Powell, Quint H., Skamser, Daniel J.
• Primary Examiner(s): THEISEN, MARY LYNN F
• Application Number:
  US09/753,026
• Publication Number:
  US 20020003225A1
• Time in Patent Office: 1,218 Days
• Field of Search: 264/7, 264/9, 264/13
• US Class Current: 264/7
• CPC Class Codes: B01J 2/003 followed by coating of the granules to prevent the granules sticking together B01J2/30
• CPC Class Codes: B01J 2/006 Coating of the granules without description of the process or the device by which the granules are obtained to prevent the granules sticking together B01J2/30
• CPC Class Codes: B01J 2/02 by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
• CPC Class Codes: B01J 2/04 in a gaseous medium if combined with suspending the material in a gas, e.g. fluidised beds B01J2/16
• CPC Class Codes: B01J 2219/00155 using insulating materials or refractories
• CPC Class Codes: B01J 2219/00159 controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
• CPC Class Codes: B01J 2219/00162 controlling the pressure
• CPC Class Codes: B01J 2219/00166 controlling the residence time inside the reactor vessel
• CPC Class Codes: B01J 2219/00171 controlling the density
• CPC Class Codes: B01J 2219/00186 controlling the composition of the reactive mixture
• CPC Class Codes: B24B 37/044 characterised by the composition of the lapping agent
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 13/185 Preparing mixtures of oxides
• CPC Class Codes: C01B 17/20 Methods for preparing sulfides or polysulfides, in general ammonium sulfides or polysulfides C01C; sulfides or polysulfides of metals, other than alkali metals, magnesium, calcium, strontium and barium, see the relevant groups of subclasses C01F or C01G, according to the metal
• CPC Class Codes: C01F 17/235 Cerium oxides or hydroxides
• CPC Class Codes: C01G 15/006 Compounds containing, besides gallium, indium, or thallium, two or more other elements, with the exception of oxygen or hydrogen
• CPC Class Codes: C01G 23/003 Titanates C01G23/001 takes precedence
• CPC Class Codes: C01G 23/006 Alkaline earth titanates
• CPC Class Codes: C01G 25/00 Compounds of zirconium
• CPC Class Codes: C01P 2002/60 Compounds characterised by their crystallite size
• CPC Class Codes: C01P 2002/70 : defined by measured X-ray, neutron or electron diffraction data
• CPC Class Codes: C01P 2004/03 : obtained by SEM
• CPC Class Codes: C01P 2004/32 : Spheres
• CPC Class Codes: C01P 2004/34 : hollow
• CPC Class Codes: C01P 2004/50 : Agglomerated particles
• CPC Class Codes: C01P 2004/52 : highly monodisperse size distribution
• CPC Class Codes: C01P 2004/61 : Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2004/62 : Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2004/80 : Particles consisting of a mixture of two or more inorganic phases
• CPC Class Codes: C01P 2006/10 : Solid density
• CPC Class Codes: C01P 2006/60 : Optical properties, e.g. expressed in CIELAB-values
• CPC Class Codes: C01P 2006/80 : Compositional purity
• CPC Class Codes: C09G 1/02 : containing abrasives or grinding agents abrasives as such C09K3/14; polishing of semi-conductors H01L
• CPC Class Codes: C09K 3/1436 : Composite particles, e.g. coated particles
• CPC Class Codes: C09K 3/1463 : Aqueous liquid suspensions
• CPC Class Codes: H01G 4/0085 : Fried electrodes
• CPC Class Codes: H01J 29/20 : characterised by the luminescent material
• CPC Class Codes: H01L 21/3212 : by chemical mechanical polishing [CMP]
• CPC Class Codes: H01L 23/49883 : the conductive materials containing organic materials or pastes, e.g. for thick films for printed circuits H05K1/092
• CPC Class Codes: H01L 2924/00 : Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
• CPC Class Codes: H01L 2924/0002 : Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Abstract

Chemical-mechanical planarization slurries and methods for using the slurries wherein the slurry includes abrasive particles. The abrasive particles have a small particle size, narrow size distribution and a spherical morphology and the particles are substantially unagglomerated.

Claims

1. A method for the production of abrasive particles adapted for use in a CMP slurry, comprising the steps of:

a) generating an aerosol of droplets from a liquid wherein said liquid comprises an abrasive compound precursor and wherein said droplets have a size distribution such that at least about 80 weight percent of said droplets have a size of not greater than about 5 μ

m;

b) moving said droplets in a carrier gas; and

c) heating said droplets to remove liquid therefrom and form abrasive particles of said abrasive compound.

2. A method as recited in claim 1, wherein said carrier gas comprises air.

3. A method as recited in claim 1, wherein said heating step comprises passing said droplets through a heating zone having a temperature of from about 400°

C. to about 1200°

C.

4. A method as recited in claim 1, wherein said abrasive particles have a particle density of at least about 90 percent of the theoretical density of said abrasive compound.

5. A method as recited in claim 1, wherein said droplets have a droplet size distribution such that no greater than about 20 weight percent of the droplets in said aerosol are larger than about twice the weight average droplet size.

6. A method as recited in claim 1, further comprising the step of removing a portion of droplets from said aerosol, wherein said removed droplets have an aerodynamic diameter greater than a preselected maximum diameter.

7. A method as recited in claim 1, wherein said liquid is an aqueous-based solution comprising an abrasive compound precursor selected from the group consisting of nitrates, hydroxides, chlorides, sulfates and oxalates.

8. A method as recited in claim 1, wherein said liquid comprises a colloidal suspension.

9. A method as recited in claim 1, further comprising the step of coating an outer surface of said abrasive particles.

10. A method as recited in claim 1, further comprising the step of coating an outer surface of said abrasive particles with a metal oxide coating.

11. A method as recited in claim 1, wherein said abrasive compound is selected from the group consisting of Al₂O₃, SiO₂, CeO₂ and ZrO₂.

12. A method as recited in claim 1, wherein said step of generating an aerosol comprises the step of using a plurality of ultrasonic transducers.

13. A method as recited in claim 1, wherein said step of generating an aerosol comprises the step of using a plurality of ultrasonic transducers having a frequency of at least about 1.7 MHz.

14. A method as recited in claim 1, wherein said liquid further comprises a densification aid.

15. A method as recited in claim 1, wherein said liquid further comprises urea.

16. A method for the production of abrasive particles adapted for use in a CMP slurry, comprising the steps of:

a) generating an aerosol of droplets from a liquid wherein said liquid comprises a silica precursor and wherein said droplets have a size distribution such that at least about 80 weight percent of said droplets have a size of not greater than about 5 μ

m;

b) moving said droplets in a carrier gas; and

c) heating said droplets to remove liquid therefrom and form abrasive particles comprising silica.

17. A method as recited in claim 16, wherein said carrier gas comprises air.

18. A method as recited in claim 16, wherein said heating step comprises passing said droplets through a heating zone having a temperature of from about 400°

C. to about 1200°

C.

19. A method as recited in claim 16, wherein said droplets have a size distribution such that no greater than about 20 weight percent of the droplets in said aerosol are larger than about twice the weight average droplet size.

20. A method as recited in claim 16, further comprising the step of removing a portion of droplets from said aerosol, wherein said removed droplets have an aerodynamic diameter greater than a preselected maximum diameter.

21. A method as recited in claim 16, wherein said liquid comprises a colloidal suspension.

22. A method as recited in claim 16, further comprising the step of coating an outer surface of said abrasive particles.

23. A method as recited in claim 16, wherein said step of generating an aerosol comprises the step of using a plurality of ultrasonic transducers having a frequency of at least about 1.7 MHz.

24. A method for the production of abrasive particles adapted for use in a CMP slurry, comprising the steps of:

a) generating an aerosol of droplets from a liquid wherein said liquid comprises an alumina precursor and wherein said droplets have a size distribution such that at least about 80 weight percent of said droplets have a size of less than about 5 μ

m;

b) moving said droplets in a carrier gas; and

c) heating said droplets to remove liquid therefrom and form abrasive particles comprising alumina.

25. A method as recited in claim 24, wherein said carrier gas comprises air.

26. A method as recited in claim 24, wherein said heating step comprises passing said droplets through a heating zone having a temperature of from about 400°

C. to about 1200°

C.

27. A method as recited in claim 24, wherein said droplets have a size distribution such that no greater than about 20 weight percent of the droplets in said aerosol are larger than about twice the weight average droplet size.

28. A method as recited in claim 24, further comprising the step of removing a portion of droplets from said aerosol, wherein said removed droplets have an aerodynamic diameter greater than a preselected maximum diameter.

29. A method as recited in claim 24, wherein said alumina precursor comprises aluminum nitrate.

30. A method as recited in claim 24, wherein said liquid comprises a colloidal suspension.

31. A method as recited in claim 24, further comprising the step of coating an outer surface of said abrasive particles.

32. A method as recited in claim 24, wherein said step of generating an aerosol comprises the step of using a plurality of ultrasonic transducers having a frequency of at least about 1.7 MHz.

33. A method for the production of abrasive compound particles adapted for use in a CMP slurry, comprising the steps of:

a) generating an aerosol of droplets from a liquid wherein said liquid comprises a ceria precursor and wherein said droplets have a size distribution such that at least about 80 weight percent of said droplets have a size of less than about 5 μ

m;

b) moving said droplets in a carrier gas; and

c) heating said droplets to remove liquid therefrom and form abrasive particles comprising ceria.

34. A method as recited in claim 33, wherein said carrier gas comprises air.

35. A method as recited in claim 33, wherein said heating step comprises passing said droplets through a heating zone having a temperature of from about 600°

C. to about 1100°

C.

36. A method as recited in claim 33, wherein said droplets have a size distribution such that no greater than about 20 weight percent of the droplets in said aerosol are larger than about twice the weight average droplet size.

37. A method as recited in claim 33, further comprising the step of removing a portion of droplets from said aerosol, wherein said removed droplets having aerodynamic diameter greater than a preselected maximum diameter.

38. A method as recited in claim 33, wherein said liquid is an aqueous-based solution comprising a ceria precursor selected from the group consisting of cerium ammonium nitrate, cerium nitrate and cerium chloride.

39. A method as recited in claim 33, wherein said liquid comprises a colloidal suspension.

40. A method as recited in claim 33, further comprising the step of coating an outer surface of said abrasive particles.

41. A method as recited in claim 33, wherein said step of generating an aerosol comprises the step of using ultrasonic transducers.

42. A method for the production of coated abrasive particles, comprising the steps of:

a) forming a liquid solution comprising an abrasive compound precursor;

b) generating an aerosol of droplets from said liquid solution;

c) moving said droplets in a carrier gas;

d) heating said droplets to remove liquid therefrom and form abrasive particles comprising said abrasive compound; and

e) coating an outer surface of said abrasive particles.

43. A method as recited in claim 42, wherein said abrasive compound is selected from the group consisting of Al₂O₃, SiO₂, CeO₂ and ZrO₂.

44. A method as recited in claim 42, wherein said coating comprises a compound selected from SiO₂ and Al₂O₃.

45. A method as recited in claim 42, wherein said coating comprises an organic compound.

46. A method as recited in claim 42, wherein said coating step comprises contacting said abrasive particles with a volatile coating precursor.

47. A method as recited in claim 42, wherein said coating step comprises contacting said metal particles with a volatile coating precursor selected from the group consisting of metal chlorides, metal acetates and metal alkoxides.

48. A method as recited in claim 42, wherein said abrasive compound precursor is a silica precursor and wherein said coating comprises alumina.

49. A method as recited in claim 42, wherein said coating is adapted to be consumed during use of said slurry in a polishing process.