HIGH PERFORMANCE COMPOSITE DIELECTRIC INK FOR ULTRACAPACITORS

• US 20170174915A1
• Filed: 12/16/2015
• Published: 06/22/2017
• Est. Priority Date: 12/16/2015
• Status: Active Grant

• Current Assignee: United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration
• Original Assignee: The United States of America As Represented By The Secretary of Agriculture
• Inventors: Rolin, Terry D., Hill, Curtis W.
• Granted Patent: US 9,745,481 B2
• Time in Patent Office: Days
• CPC Class Codes: C08K 2003/2206 of calcium, strontium or barium
• CPC Class Codes: C08K 2003/2237 of titanium
• CPC Class Codes: C08K 2201/003 Additives being defined by their diameter
• CPC Class Codes: C08K 2201/011 Nanostructured additives
• CPC Class Codes: C08K 3/22 of metals
• CPC Class Codes: C08K 3/24 Acids; Salts thereof C08K3/16 takes precedence
• CPC Class Codes: C08K 3/40 Glass
• CPC Class Codes: C08K 9/02 Ingredients treated with inorganic substances
• CPC Class Codes: C09D 11/033 characterised by the solvent
• CPC Class Codes: C09D 11/037 characterised by the pigment
• CPC Class Codes: C09D 11/14 based on carbohydrates
• CPC Class Codes: C09D 11/322 Pigment inks
• CPC Class Codes: C09D 11/36 based on non-aqueous solvents
• CPC Class Codes: H01G 13/04 Drying; Impregnating
• CPC Class Codes: H01G 4/12 Ceramic dielectrics H01G4/085 takes precedence
• CPC Class Codes: H01G 4/129 containing a glassy phase, e.g. glass ceramic
• CPC Class Codes: H01G 4/30 Stacked capacitors H01G4/33 takes precedence
• CPC Class Codes: H01G 4/33 Thin- or thick-film capacitors thin- or thick-film circuits H01L27/00; capacitors without a potential-jump or surface barrier specially adapted for integrated circuits, details thereof, multistep manufacturing processes therefor H01L28/40
• CPC Class Codes: H05K 1/162 incorporating printed capacitors
• CPC Class Codes: H05K 2201/0179 Thin film deposited insulating layer, e.g. inorganic layer for printed capacitor
• CPC Class Codes: H05K 2201/0209 : Inorganic, non-metallic particles
• CPC Class Codes: H05K 2203/0776 : Uses of liquids not otherwise provided for in H05K2203/0759 - H05K2203/0773
• CPC Class Codes: Y02E 60/13 : Energy storage using capacitors

Abstract

The present invention is a dielectric ink and means for printing using said ink. Approximately 10-20% of the ink is a custom organic vehicle made of a polar solvent and a binder. Approximately 30-70% of the ink is a dielectric powder having an average particle diameter of approximately 10-750 nm. Approximately 5-15% of the ink is a dielectric constant glass. Approximately 10-35% of the ink is an additional amount of solvent. The ink is deposited on a printing substrate to form at least one printed product, which is then dried and cured to remove the solvent and binder, respectively. The printed product then undergoes sintering in an inert gas atmosphere.

Claims

1. A ultracapacitor, comprised of:

(a) at least one printing substrate for receiving a deposition of dielectric material to form at least one printed structure for an ultracapacitor;

(b) a high-temperature dielectric ink composition, comprised of a custom organic vehicle comprised of a polar solvent and a binder

i. wherein said polar solvent comprises approximately 50% to approximately 80% of said custom organic vehicle,

ii. wherein said binder comprises approximately 20% to approximately 50% of said custom organic vehicle,

iii. wherein said custom organic vehicle comprises approximately 10% to approximately 20% of said dielectric ink composition;

(c) a dielectric powder having an average particle diameter ranging from approximately 10 nm to approximately 750 nm, wherein said dielectric powder comprises approximately 30% to approximately 70% of said dielectric ink composition;

(d) a dielectric constant glass, wherein said dielectric constant glass does not affect the Curie temperature of the dielectric powder during sintering and comprises approximately 5% to approximately 15% of said dielectric ink composition;

(e) an additional amount of said polar solvent, wherein said additional amount of said polar solvent comprises approximately 10% to approximately 35% of said dielectric ink composition.

2. The composition of claim 1, wherein said polar solvent is selected from the group consisting of:

2,2,4-trimethyl-1,3-pentandiol monoisobutyrate, terpineol and diethylene glycol monobutyl ether.

3. The composition of claim 1, wherein said binder comprises ethyl cellulose.

4. The composition of claim 1, wherein said dielectric powder is perovskite.

5. The composition of claim 1, wherein said dielectric powder is doped.

6. The composition of claim 1, wherein particles of said dielectric powder have a coating of silica approximately 5 nm to approximately 10 nm thick.

7. The composition of claim 1, wherein said dielectric powder has a dielectric constant ranging from approximately 5,000 to approximately 1.4 million.

8. The composition of claim 1, wherein said dielectric constant glass is selected from the group consisting of:

lead-germanate glass.

9. The composition of claim 1, wherein said dielectric constant glass has a dielectric constant of up to approximately 10.

10. The composition of claim 1 further comprising a dispersant, wherein said dispersant comprises approximately 0.5% to approximately 5% of said dielectric ink composition.

11. A method of preparing a dielectric ink composition for an ultracapacitor, comprising the steps of:

(a) preparing a custom organic vehicle by combining approximately 50% to approximately 80% polar solvent and approximately 20% to approximately 50% binder material, wherein said custom organic vehicle comprises approximately 10% to approximately 20% of said dielectric ink composition;

(b) combining a dielectric powder having an average particle diameter ranging from approximately 50 nm to approximately 750 nm with said custom vehicle, wherein said custom organic vehicle comprises approximately 50% to approximately 70% of said dielectric ink composition;

(c) combining a dielectric constant glass with said dielectric powder and said custom organic vehicle, wherein said dielectric constant glass comprises approximately 5% to approximately 15% of said dielectric ink and wherein said dielectric constant glass does not affect the Curie temperature of the dielectric powder during sintering composition; and

(d) combining an additional quantity of said polar solvent with said dielectric constant glass, said dielectric powder and said custom vehicle, wherein said additional quantity of said polar solvent comprises approximately 10% to approximately 35% of said dielectric ink composition.

12. The method of claim 11, further comprising the step of adding a dispersant to said dielectric ink composition until said dispersant comprises up to 5% of said dielectric ink composition.

13. The method of claim 11, wherein said additional quantity of said polar solvent, said dielectric constant glass, said dielectric powder and said custom vehicle are combined using a means selected from the group consisting of:

a three-roll mill and a high-shear mixer.

14. A method of printing with a dielectric ink composition, comprising the steps of:

(a) utilizing a means of deposition to deposit said dielectric ink composition on a printing substrate to form at least one printed product for an ultracapacitor, wherein said dielectric ink composition is comprised of;

i. a custom organic vehicle comprised of a polar solvent and a binder, wherein said polar solvent comprises approximately 50% to approximately 80% of said custom organic vehicle, wherein said binder comprises approximately 20% to approximately 50% of said custom organic vehicle, wherein said custom organic vehicle comprises approximately 10% to approximately 20% of said dielectric ink composition,

ii. a dielectric powder having an average particle diameter ranging from approximately 50 nm to approximately 750 nm, wherein said dielectric powder comprises approximately 50% to approximately 70% of said dielectric ink composition,

iii. a dielectric constant glass, wherein said dielectric constant glass comprises approximately 5% to approximately 15% of said dielectric ink composition wherein said dielectric constant glass does not affect the Curie temperature of the dielectric powder during sintering, and an additional amount of said polar solvent, wherein said additional amount of said polar solvent comprises approximately 10% to approximately 35% of said dielectric ink composition;

(b) drying said at least one printed product to remove said polar solvent from said dielectric ink composition;

(c) curing said at least one printed product to remove said binder from said dielectric ink composition; and

(d) sintering said at least one printed product in an inert gas atmosphere.

15. The method of claim 14, wherein said means of deposition is selected from the group consisting of:

aerosol deposition, inkjet deposition, screen-printing and three-dimensional printing.

16. The method of claim 14, wherein said inert gas atmosphere is a nitrogen atmosphere.

17. The method of claim 16, wherein said nitrogen gas atmosphere comprises less than 5 PPM of impurities.

18. The method of claim 14, wherein said step of sintering takes place at a maximum of 1,200 degrees C. for approximately 10 minutes to approximately 15 minutes.

19. The method of claim 14, wherein said step of sintering heats said printed product at a rate ranging from approximately 45 degrees C./minute to approximately 55 degrees C./minute, wherein said step of sintering cools said printed product at a rate ranging from approximately 45 degrees C./minute to approximately 55 degrees C./minute.

20. The method of claim 14, wherein said at least one printed product is a solid-state ultracapacitor.