1. A method for preparing polyurea compounds by reacting amines and isocyanates in the presence of a liquid diluent in a high-pressure impingement mixing device under conditions sufficient to produce a polyurea compound having the consistency of a powder and in which diluent is dispersed.
2. The method of claim 1 wherein the liquid diluent is simultaneously mixed with the amines and isocyanates wherein each component exhibits substantially similar densities.
3. The process of claim 2 wherein the liquid diluent is inert to the amines and isocyanate.
4. The process of claim 3 wherein the diluent is chosen from the group consisting of naphthenic, paraffinic, PAO, ester, PAG, carbon base solvents and any combination thereof.
5. The process of claim 4 wherein the ratio of diluent to amine is in the range of about 1:1 to about 3:1.
6. The process of claim 5 wherein the amines and isocyanates are fed to the impingement device in a mole ratio of about 1:1 to about 2:1, at a temperature in the range of about 0\xb0 C. to about 100\xb0 C. and a pressure above about 500 psig through reactor orifices having an orifice of from about 0.030 to about 0.109.
7. The process of claim 6 wherein the particles are passed through a containment zone equipped with FTIR monitoring means.
8. The process of claim 7 including process control means operably connected to the monitoring means for adjusting processing conditions when necessary to maintain substantially complete reaction.
9. A polyurea thickened grease comprising a base oil and a polyurea thickener prepared by the process of claim 6.
10. A method for making a particulate polyurea composition that can be homogenized into a grease at standard grease homogenizing conditions, the method comprising feeding a solution of an amine or isocyanate and a lubricating medium or solvent into an impingement reactor (mix chamber) while feeding a isocyanine into the reactor, wherein the mole ratio of amine to isocyanate is in the range of about 1:1 to about 2:1 whereby a polyurea particulate composition having a powdery consistency is produced that can be homogenized into a grease under grease forming conditions at standard homogenizing conditions.
11. The method of claim 10 wherein the weight ratio of lubricating medium or solvent to component (reactants) is in the range of about 1:5 to about 1:3.
12. The method of claim 11 wherein the feeding of individual component or component solutions is conducted at pressures of from about 1000 psi to about 1800 psi.
13. The method of claim 12 wherein the feeding is conducted at temperatures in the range of from about 24\xb0 C. to about 55\xb0 C.
14. A method for forming a grease comprising:
mixing a base lubricating oil and a polyurea prepared by the methods of claims 10, 11, 12 and 13;
heating the mixture of base oil and polyurea to a temperature in the range of about 150\xb0 C. to about 175\xb0 C.; and
thereafter milling the heated mixture to form a homogenized grease.
15. The method of claim 1 wherein the isocyanate is a diisocyanate.
16. The method of claim 10 wherein the isocyanate is a diisocyanate.
17. A polyurea particle with a density of less than 6.5 lbsgal.
18. A polyurea particle with a specific surface area of more than 20 m2g.
19. A polyurea particle that is at least between 10 microns and less than 700 microns, a density of less than 6.5 lbsgal, and a specific surface area of more than 20 m2g.
20. A polyurea particle that is at least between 10 microns and less than 700 microns, a density of less than 5.75 lbsgal, and a specific surface area of more than 32 m2g.
21. A polyurea grease comprising a polyurea particle that is at least between 10 microns and less than 700 microns, a density of less than 6.5 lbsgal, and a specific surface area of more than 20 m2g, the polyurea particle blended with a lubricating oil.
22. A polyurea grease comprising a polyurea particle that is at least between 10 microns and less than 700 microns, a density of less than 6.5 lbsgal, and a specific surface area of more than 20 m2g, the polyurea particle blended with a lubricating oil.
The claims below are in addition to those above.
All refrences to claim(s) which appear below refer to the numbering after this setence.
1. A manufacturing method of a semiconductor device, comprising:
providing a low-relative-dielectric-constant film above a substrate, the low-relative-dielectric-constant film containing at least oxygen (O) and having a relative dielectric constant of 3.3 or more, a conductor being to be buried in the low-relative-dielectric-constant film;
performing a plasma processing by discharging a gas containing a noble gas as a main component to the low-relative-dielectric-constant film, the plasma processing being executed while the substrate above which the low-relative-dielectric-constant film is provided is storing in a processing chamber having an inside covered with a material composed of an element except for oxygen and substantially set under an oxygen-free atmosphere; and
providing a first insulating film above the low-relative-dielectric-constant film by a plasma CVD method, the first insulating film being made of a material containing at least one of a material containing oxygen and a material containing an element reacting with oxygen, a conductor being to be buried in the first insulating film.
2. The method according to claim 1, further comprising:
providing a second insulating film on the low-relative-dielectric-constant film before the first insulating film is provided, the second insulating film being made of an element except for oxygen, a conductor being to be buried in the second insulating film, and the second insulating film being provided in the processing chamber while performing the plasma processing to the low-relative-dielectric-constant film, keeping the substrate above which the low-relative-dielectric-constant film is provided is under an oxygen-free atmosphere until formation of the second insulating film is finished.
3. The method according to claim 1, wherein
the low-relative-dielectric-constant film is formed by using a material containing oxygen (O) and at least one element of silicon (Si), carbon (C), and hydrogen (H).
4. The method according to claim 1, wherein
the first insulating film is formed by using a material at least containing at least one of oxygen and an element reacting with oxygen, and silicon (Si).
5. The method according to claim 1, wherein
the plasma processing is performed in another processing chamber different from a processing chamber using to provide the low-relative-dielectric-constant film.
6. The method according to claim 1, wherein
the plasma processing is performed by using a gas containing at least one element of argon (Ar), helium (He), neon (Ne), krypton (Kr), xenon (Xe), and radon (Rn) as a main component.
7. The method according to claim 1, wherein
the plasma processing is performed more than once by using gases of different types containing different noble gas elements as main components.
8. The method according to claim 1, wherein
the plasma processing is performed at about 450\xb0 C. or less.
9. The method according to claim 2, wherein
the inside of the processing chamber is covered with the same material as that of the second insulating film before the second insulating film is provided.
10. The method according to claim 2, wherein
the inside of the processing chamber is covered with a material containing silicon (Si) and at least one of carbon (C) and nitrogen (N) before the second insulating film is provided.
11. A manufacturing method of a semiconductor device, comprising:
providing a first low-relative-dielectric-constant film above a substrate, the first low-relative-dielectric-constant film containing at least oxygen (O), and having a relative dielectric constant of 3.3 or less, a conductor being to be buried in the first low-relative-dielectric-constant film;
providing a second low-relative-dielectric-constant film on the first low-relative-dielectric-constant film, the second low-relative-dielectric-constant film containing at least oxygen (O), having a relative dielectric constant of 3.3 or less and having a film density higher than that of the first low-relative-dielectric-constant film, a conductor being to be buried in the second low-relative-dielectric-constant film; and
irradiating an electron beam on at least the first and second low-relative-dielectric-constant films.
12. The method according to claim 11, further comprising:
providing a first insulating film above the second low-relative-dielectric-constant film by a plasma CVD method after the electron beam is irradiated on the first and second low-relative-dielectric-constant films, the first insulating film being made of a material containing at least one of oxygen and an element reacting with oxygen, a conductor being to be buried in the first insulating film.
13. The method according to claim 11, further comprising:
providing a third low-relative-dielectric-constant film on the second low-relative-dielectric-constant film by a coating method before the electron beam is irradiated on the first and second low-relative-dielectric-constant films, the third low-relative-dielectric-constant film having a relative dielectric constant of 3.3 or less, and the electron beam being irradiating on the first, second, and third low-relative-dielectric-constant films after the third low-relative-dielectric-constant film is provided on the second low-relative-dielectric-constant film.
14. The method according to claim 11, wherein
the first and second low-relative-dielectric-constant films are formed by using a material containing oxygen (O) and at least one element of silicon (Si), carbon (C), and hydrogen (H).
15. The method according to claim 11, wherein
the substrate provided the first low-relative-dielectric-constant film there above is kept under an oxygen-free atmosphere at least until completing the formation of the second low-relative-dielectric-constant film.
16. The method according to claim 11, wherein
the electron beam irradiation is performed at about 450\xb0 C. or less.
17. The method according to claim 12, wherein
the first insulating film is formed by using a material at least containing at least one of oxygen and an element reacting with oxygen, and silicon (Si).
18. The method according to claim 12, further comprising:
providing a second insulating film on the second low-relative-dielectric-constant film before the first insulating film is provided, the second insulating film being made of an element except for oxygen, a conductor being to be buried in the second insulating film.
19. The method according to claim 18, wherein
the second insulating film is provided while performing a plasma processing to the second low-relative-dielectric-constant film in a processing chamber having an inside covered with a material containing silicon (Si) and at least one of carbon (C) and nitrogen (N) and substantially set under an oxygen-free atmosphere.
20. The method according to claim 13, wherein
the third low-relative-dielectric-constant film is formed by an organic resin.