Method of accurate thickness measurement of boron carbide coating on copper foil

• US 9,810,635 B2
• Filed: 11/12/2015
• Issued: 11/07/2017
• Est. Priority Date: 11/12/2014
• Status: Active Grant

• Current Assignee: Proportional Technologies, Inc.
• Original Assignee: Proportional Technologies, Inc.
• Inventors: Lacy, Jeffrey L., Regmi, Murari
• Primary Examiner(s): PHAM, HOA Q
• Application Number:
  US14/938,903
• Publication Number:
  US 20160161416A1
• Time in Patent Office: 726 Days
• Field of Search: 356630-632, 356318, 356432-440
• CPC Class Codes: G01N 2021/8427 Coatings
• CPC Class Codes: G01N 21/68 using high frequency electric fields
• CPC Class Codes: G01N 21/73 using plasma burners or torches

Abstract

A method is disclosed of measuring the thickness of a thin coating on a substrate comprising dissolving the coating and substrate in a reagent and using the post-dissolution concentration of the coating in the reagent to calculate an effective thickness of the coating. The preferred method includes measuring non-conducting films on flexible and rough substrates, but other kinds of thin films can be measure by matching a reliable film-substrate dissolution technique. One preferred method includes determining the thickness of Boron Carbide films deposited on copper foil. The preferred method uses a standard technique known as inductively coupled plasma optical emission spectroscopy (ICPOES) to measure boron concentration in a liquid sample prepared by dissolving boron carbide films and the Copper substrates, preferably using a chemical etch known as ceric ammonium nitrate (CAN). Measured boron concentration values can then be calculated.

Claims

1. A process for measuring the effective thickness of a boron coating on copper foil comprising the steps of:

(1) removing a sample of the boron coated copper foil from a larger length coated substrate;

(2) weighing the sample of boron coated copper foil;

(3) contacting the sample of boron coated copper foil with an etching solution;

(4) allowing the etching solution to dissolve the sample of boron coated copper foil;

(5) diluting the etching solution;

(6) determining the concentration of the material in the diluted etching solution utilizing inductively coupled plasma optical emission spectroscopy; and

(7) calculating the effective thickness of the coating (t_s) using the equation;

t_s=[(1.3C×

V_s×

d_f×

t_cu×

d_cu/M_t)×

1/(1−

1.3C×

V_s×

d_f/M_t)]

where C=measured concentration from determining step

d_f=sample dilution factor

V_s=volume of diluted etching solution

t_cu=thickness of the copper foil

dcu—

density of the copper foil

Mt=mass of the boron coated sample.

2. The process of claim 1, wherein the removing a sample step comprises removing a sample at least about 1 square centimeter in size.

3. The process of claim 1, wherein the removing step comprises removing multiple samples from the substrate, the samples being taken at intervals of between about 50 and about 200 feet along the substrate.

4. The process of claim 1, wherein the boron coating comprises a boron carbide coating.

5. The process of claim 1 wherein the etching solution of the contacting step comprises a ceric ammonium nitrate solution.

6. The process of claim 5, wherein the ceric ammonium nitrate solution comprises between about 2 and about 25 percent by weight ceric ammonium nitrate.

7. The process of claim 5, wherein the ceric ammonium nitrate solution comprises between about 8 and about 10 percent by weight ceric ammonium nitrate.

8. The process of claim 1, wherein the diluting step comprises diluting the boron concentration to between about 2 and about 25 ppm.

9. The process of claim 1, wherein the determining the concentration step comprises determining the boron concentration to within about 0.1 ppm.

10. A process for measuring the effective thickness of a boron carbide coating on copper foil comprising the steps of:

(1) removing a sample of the boron carbide coated copper foil from a larger length of boron carbide coated copper foil;

(2) weighing the sample of boron carbide coated copper foil;

(3) contacting the sample of boron carbide coated copper foil with ceric ammonium nitrate etching solution;

(4) allowing the etching solution to dissolve the sample of boron carbide coated copper foil;

(5) diluting the etching solution to between about 2 and about 25 ppm boron;

(6) determining the concentration of boron carbide in the diluted etching solution using inductively coupled plasma optical emission spectroscopy; and

(7) calculating the effective thickness of the boron coating (t_s) using the equation;

t_s=[(1.3C×

V_s×

d_f×

t_cu×

d_cu/M_t)×

1/(1−

1.3C×

V_s×

d_f/M_t)]

where C=measured concentration from determining step

d_f=sample dilution factor

V_s=volume of liquid sample prepared

t_cu=thickness of the copper foil

d_cu—

density of the copper foil

M_t=mass of the sample.

11. The process of claim 10, wherein the removing a sample step comprises removing a sample at least about 1 square centimeter in size.

12. The process of claim 10, wherein the removing step comprises removing multiple samples from the substrate, the samples being taken at intervals of between about 50 and about 200 feet along the substrate.

13. The process of claim 10, wherein the ceric ammonium nitrate solution comprises between about 2 and about 25 percent by weight ceric ammonium nitrate.

14. The process of claim 10, wherein the ceric ammonium nitrate solution comprises between about 8 and about 10 percent by weight ceric ammonium nitrate.