Methods of adjusting carbon and silica content in rice hull ash (RHA) byproducts to control carbothermal reduction forming nanostructured silicon carbide, silicon nitride, silicon oxynitride nanocomposites

Patent metadata

Field	Value
Publication number	US-12506144-B2
Application number	US-202218689910-A
Country	US
Kind code	B2
Filing date	Sep 8, 2022
Priority date	Sep 8, 2021
Publication date	Dec 23, 2025
Grant date	Dec 23, 2025

Abstract

In various aspects, methods of making a silicon carbide or silicon nitride from rice hull ash (RHA) byproduct are provided. A treated silica depleted rice hull ash product (SDRHA) comprising silicon oxide at ≤about 65% by weight and carbon ≥about 35% by weight may be heated in an environment free of any additional carbon sources, but in an inert atmosphere, having a temperature of ≥about 1,200° C. to ≤about 1,700° C. for a carbothermal reaction that forms a product (e.g., nanocomposite product) comprising at least one of silicon carbide (SiC), silicon nitride (Si 3 N 4 ), and silicon oxynitride (Si 2 N 2 O or non-stoichiometric SiN x O 4-x , where x ranges from greater than 0 to less than 4). A negative electroactive material is also provided that includes silicon oxynitride (Si 2 N 2 O), which may be used in a lithium ion battery.

First claim

What is claimed is:

1 . A method of making a silicon carbide or silicon nitride from rice hull ash (RHA) byproduct, the method comprising:
removing silicon oxide from a rice hull ash (RHA) byproduct to form a silica depleted rice hull ash (SDRHA) by reacting the rice hull ash (RHA) with a hindered diol in the presence of a catalytic base; heating the silica depleted rice hull ash product (SDRHA) comprising silicon oxide at less than or equal to about 65% by weight and carbon at greater than or equal to about 35% by weight in an environment free of any additional carbon sources, comprising an inert atmosphere, and having a temperature of greater than or equal to about 1,200°C to less than or equal to about 1,700°C for a carbothermal reaction that forms a product comprising at least one of silicon carbide (SiC), silicon nitride (Si 3 N 4 ), and silicon oxynitride (Si 2 N 2 O).

2 . The method of claim 1 , wherein the silica depleted rice hull ash (SDRHA) comprises greater than or equal to about 35% by weight to less than or equal to about 60% by weight of carbon.

3 . The method of claim 1 , wherein the silica depleted rice hull ash (SDRHA) has a ratio of SiO 2 to carbon (SiO 2 :C) of about 1:8 to about 1:3.

4 . The method of claim 1 , wherein the hindered diol is selected from the group consisting of: 2-methyl-2,4-pentanediol, 2,2,4-trimethyl-1,3-pentanediol, and combinations thereof.

5 . The method of claim 1 , wherein the catalytic base is selected from the group consisting of: sodium hydroxide (NaOH), lithium hydroxide (LiOH), calcium hydroxide Ca(OH) 2 , potassium hydroxide (KOH), cesium hydroxide (CsOH), rubidium hydroxide (RbOH), and combinations thereof.

6 . The method of claim 1 , wherein the hindered diol comprises 2-methyl-2,4-pentanediol and the catalytic base comprises sodium hydroxide (NaOH).

7 . The method of claim 1 , wherein the temperature is greater than or equal to about 1,400° C. to less than or equal to about 1,600° C.

8 . The method of claim 1 , wherein the product is a nanocomposite.

9 . The method of claim 1 , wherein the product comprises greater than or equal to about 75% by weight silicon carbide (SiC).

10 . The method of claim 1 , wherein the product comprises a nanocomposite with a phase comprising silicon oxynitride (SiN x O 4-x , where x ranges from greater than 0 to less than 4) having nanostructures comprising at least one of silicon carbide (SiC) and silicon nitride (Si 3 N 4 ) distributed therein.

11 . The method of claim 1 , wherein the removing silicon oxide from a rice hull ash comprises milling the rice hull ash (RHA) byproduct with an acidic solution to yield a purified rice hull ash (RHA) byproduct; and removing silicon oxide from the purified rice hull ash (RHA) byproduct by reacting the purified rice hull ash (RHA) with a hindered diol in the presence of a catalytic base to form the silica depleted rice hull ash (SDRHA).

12 . The method of claim 11 , further comprising after the milling, washing the purified rice hull ash (RHA) byproduct with boiling water to remove impurities.

Assignees

• Univ Michigan Regents

Inventors

• Yu Mengjie
• Laine Richard
• Temeche Eleni

Classifications

• C01B32/97

  Preparation from SiO or SiO2 · CPC title

• H01B1/04

  mainly consisting of carbon-silicon compounds, carbon or silicon · CPC title

• Y02E60/10

  Energy storage using batteries · CPC title

• H01M2004/027

  Negative electrodes · CPC title

• H01M4/0471

  involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis · CPC title