# US 11,993,693 B2 · Composite of non-polar organic polymer and ultra-low-wettability carbon black

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- Number: US 11,993,693 B2
- Document ID: US11993693B2
- Status: Granted
- Kind: B2
- Application number: 16/976,509
- Filed: 2019-03-22
- Published: 2021-01-07
- Granted: 2024-05-28
- Earliest claimed: 2018-03-28
- Assignees: Dow Global Technologies LLC; Rohm and Haas Company
- Applicants: Dow Global Technologies LLC; Rohm and Haas Company
- Inventors: Tian Lan; Xindi Yu; Michael Q. Tran; Paul J. Brigandi; Jeffrey M. Cogen; Timothy J. Person; Yichi Zhang
- Web page: https://patentgrep.com/patent/US11993693B2

## CPC

- C08K 3/04: Carbon
- C08F 10/02: Ethene
- C08J 3/201: {Pre-melted polymers}
- H01B 3/22: hydrocarbons
- H01B 7/0275: {comprising one or more extruded layers of insulation}
- C08F 2810/20: leading to a crosslinking, either explicitly or inherently
- C08K 2201/001: Conductive additives
- C08K 2201/006: Additives being defined by their surface area
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K})

## Abstract

A semiconductive composite material consisting essentially of a non-polar organic polymer and an electrical conducting effective amount of an ultra-low-wettability carbon black. Also a method of making the composite material; a crosslinked polyethylene product made by curing the composite material; manufactured articles comprising a shaped form of the inventive composite material or product; and methods of using the inventive composite material, product, or articles.

## Claims

### Claim 1

A semiconductive composite material consisting essentially of (A) a non-polar polyolefin polymer and an electrical conducting effective amount of (B) an ultra-low-wettability carbon black (ULW-CB), which has a Brunauer-Emmett-Teller (BET) nitrogen surface area of from 35 to 190 square meters per gram (m2/g), measured by BET Nitrogen Surface Area Test Method; and an oil absorption number (OAN) from 115 to 180 milliliters of oil per 100 grams (mL/100 g), measured by Oil Absorption Number Test Method according to ASTM D2414-04 using Procedure A with dibutyl phthalate (DBP); and a water uptake of from 400 to 2400 parts per million (ppm, weight), measured by Moisture Uptake Test Method,
wherein the BET Nitrogen Surface Area Test Method is performed using a Micromeritics Accelerated Surface Area & Porosimetry instrument (ASAP 2420) that out-gases samples at 250° C.,
wherein the Moisture Uptake Test Method is preformed by drying a carbon black sample in a vacuum oven at 100° C. overnight, measuring the weight of the dried carbon black sample, placing the dried carbon black sample inside a chamber with well-controller 80% relative humidity (RH) and temperature 24° C. for 24 hours to give a humidified carbon black sample, weighing the humidified carbon black sample, and calculating the amount of moisture uptake in weight parts per million using the following equation; amount moisture uptake=(weight of humidified CB sample-weight of dried CB sample) divided by weight of dried CB sample.

### Claim 2 (depends on 1)

The semiconductive composite material of claim 1 wherein the (B) ULW-CB is characterized by any one of limitations (i) to (iii): (i) the BET nitrogen surface area is from 40 to 63 m2/g; (ii) the BET nitrogen surface area from 120 to 180 m2/g; and (iii) the (B) ULW-CB is a blend of the ULW-CBs of (i) and (ii).

### Claim 3

A semiconductive composite material consisting essentially of (A) a non-polar polyolefin polymer and an electrical conducting effective amount of (B) an ultra-low-wettability carbon black (ULW-CB), which has a surface wettability profile characterized by wettability ≤0.0101 at surface coverage of 0.02, and wettability ≤0.0101 at surface coverage of 0.04, and wettability ≤0.0099 at surface coverage of 0.06, and wettability ≤0.0111 at surface coverage of 0.08, and wettability ≤0.0113 at surface coverage of 0.10, measured by inverse gas chromatography (IGC) according to Wettability Test Method; and a water uptake of from 400 to 2400 parts per million (ppm, weight), measured by Moisture Uptake Test Method,
wherein the Moisture Uptake Test Method is preformed by drying a carbon black sample in a vacuum over at 100° C. overnight, measuring the weight of the dried carbon black sample placing the dried carbon black sample inside a chamber with well-controlled 80% relative humidity (RH) and temperature 24° C. for 24 hours to give a humidified carbon black sample, weighing the humidified carbon black sample, and calculate the amount of moisture uptake in weight parts per million using the following equation; amount moisture uptake=(weight of humidified CB sample-weight of dried CB sample) divided by weight of dried CB sample,
wherein the Wettability Test Method is preformed using an IGC Surface Energy Analyzer instrument and the following steps; pack approximately 10 to 20 milligrams (mg) of amount of a test sample of neat carbon black into individual silanized glass column (300 mm long by 4 mm inner diameter, precondition the carbon black-packed columns for 2 hours at 100° C. and 0% relative humidity with helium carrier gas to normalize samples, perform measurements with 10 standard cable centimeter per minute (sccm) total flow rate of helium, and use methane for dead volume corrections, measure components at 100° C. and 0% relative humidity.

### Claim 4 (depends on 1)

The semiconductive composite material of claim 1 wherein the BET nitrogen surface area of the (B) ULW-CB is from 40 to 180 m2/g.

### Claim 5 (depends on 1)

The semiconductive composite material of claim 1 that is free of any carbon black other than the ultra-low-wettability carbon black.

### Claim 6 (depends on 1)

The semiconductive composite material of claim 1 characterized by any one of limitations (i) to (v): (i) consisting essentially of from 61.0 to 99.0 wt % of the (A) non-polar polyolefin polymer; and from 39.0 to 1.0 wt % of the (B) ULW-CB; based on total weight of the semiconductive material; (ii) the (A) non-polar polyolefin polymer is a non-polar ethylene-based polymer; (iii) both (i) and (ii); (iv) the (A) non-polar polyolefin polymer is a non-polar propylene-based polymer; and (v) both (i) and (iv).

### Claim 7 (depends on 1)

The semiconductive composite material of claim 1, further consisting essentially of at least one additive chosen from: (C) a plastomer; (D) an antioxidant; (E) an organic peroxide; (F) a scorch retardant; (G) an alkenyl-functional coagent; (H) a nucleating agent; (I) a processing aid; (J) an extender oil; (K) a stabilizer.

### Claim 8 (depends on 1)

A crosslinked polyethylene product that is a product of curing the semiconductive composite material of claim 1.

### Claim 9 (depends on 1)

A manufactured article comprising a shaped form of the semiconductive composite material of claim 1.

### Claim 10 (depends on 1)

An electrical conductor device comprising a conductive core and a semiconductive layer at least partially covering the conductive core, wherein at least a portion of the semiconductive layer comprises the semiconductive composite material of claim 1.

### Claim 11 (depends on 10)

A method of conducting electricity, the method comprising applying a voltage across the conductive core of the electrical conductor device of claim 10 so as to generate a flow of electricity through the conductive core.

### Claim 12 (depends on 1)

A thermally cycled semiconductive composite material made by subjecting the semiconductive composite material of claim 1 to a thermal cycle comprising heating the semiconductive composite material to from 170° to 190° C. for 1 to 5 minutes, and then cooling to 30° C. to give a cooled, thermally cycled semiconductive composite material.