Millimeter-Sized sp3 Amorphous Carbon via HTHP Treatment

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Solution Overview

Problem

Current methods fail to produce millimeter-sized bulk amorphous carbon materials with high sp3 content due to limitations in synthesis technology, resulting in small sample sizes and incomplete characterization of structure and properties.

Innovation Solution

A method involving high-temperature and high-pressure (HTHP) treatment of C60 powder using a large-volume press at specific pressure and temperature conditions to produce millimeter-sized bulk sp3 amorphous carbon, allowing for tuning of sp3 content and adjustment of mechanical, optical, and thermal properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If conventional HTHP methods are used to synthesize amorphous carbon, then sp3 content can be increased, but sample size remains limited to micrometer scale

Engineering Contradiction:
Improvesp3 contentVSAvoidsample size
Core Design Contradiction:
Quantity of substanceVSVolume of moving object

Solution Approach 1:

The patent changes the pressure parameter from conventional HTHP methods to ultra-high pressure (50-70 GPa), which enables both high sp3 content (up to 100%) and millimeter-scale sample size simultaneously. This parameter change resolves the contradiction by finding an optimal pressure range that achieves both goals.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent transitions from micrometer-scale samples to millimeter-scale bulk materials, representing a dimensional change in sample size. This allows for complete structural and property characterization while maintaining high sp3 content, resolving the contradiction between quantity of substance and volume.

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

2Stability of the object's composition

If high pressure and temperature are applied to transform carbon structure, then sp3 hybridization increases, but sample size remains too small for complete characterization

Engineering Contradiction:
Improvesp3 hybridizationVSAvoidsample size for characterization
Core Design Contradiction:
Stability of the object's compositionVSManufacturing precision

Solution Approach 1:

By applying ultra-high pressure (50-70 GPa) and controlling temperature (700-1830 K), the patent achieves complete sp3 hybridization while producing millimeter-sized samples. This parameter change enables both structural stability and sufficient sample size for comprehensive characterization.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses C60 fullerene as a precursor material before HTHP treatment. This preliminary selection of precursor ensures that the transformation process yields both high sp3 content and adequate sample size, avoiding the need for post-synthesis enlargement.

Inventive Principle:
Principle #10Preliminary action

3Stress or pressure

If diamond anvil cell or small-volume press is used, then high pressure treatment is achieved, but sample size is limited to micrometers

Engineering Contradiction:
Improvepressure treatmentVSAvoidsample size
Core Design Contradiction:
Stress or pressureVSVolume of moving object

Solution Approach 1:

The patent introduces a large-volume press as an intermediary device that can generate ultra-high pressure (50-70 GPa) while accommodating millimeter-sized samples. This mediator overcomes the volume limitation of diamond anvil cells while maintaining the high pressure capability needed for sp3 transformation.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent changes the pressure parameter to ultra-high range (50-70 GPa) and uses large-volume press technology, enabling simultaneous achievement of high pressure treatment and millimeter-scale sample production, resolving the contradiction between stress application and sample volume.

Inventive Principle:
Principle #35Parameter changes

4Ease of manufacture

If conventional synthesis methods are used, then processing is simpler, but sp3 content and structural quality are insufficient

Engineering Contradiction:
Improvesynthesis process simplicityVSAvoidsp3 content
Core Design Contradiction:
Ease of manufactureVSQuantity of substance

Solution Approach 1:

The patent applies ultra-high pressure (50-70 GPa) and specific temperature ranges (700-1830 K) to transform C60 into sp3 amorphous carbon. While the pressure parameter is extreme, the use of C60 as precursor and large-volume press technology maintains relative process simplicity while achieving superior sp3 content (up to 100%).

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method successfully synthesizes millimeter-sized bulk sp3 amorphous carbon with sp3 content exceeding 80%, achieving ultra-high hardness, high thermal conductivity, and tunable optical band gaps, overcoming previous limitations in sample size and property characterization.

Implementation Method 1

performing an HTHP treatment on a sample of C60 powder at a temperature of 450-1100°C., and a pressure of 20-37 GPa

Methodology Applied
Scientific EffectHigh-temperature and high-pressure (HTHP) treatment: Pressure Increase

Implementation Method 2

The orbitals occupied by the electrons in the outer layer of carbon atoms can be hybridized in various forms such as to form sp, sp2, and sp3 hybrid bonds

Methodology Applied
Scientific Effectsp3 hybridization: Chemical Bonding

Implementation Method 3

a method for synthesizing the bulk sp3 amorphous carbon material by using a large-volume press

Methodology Applied
Scientific EffectCompression: Compression

Implementation Method 4

performing an HTHP treatment on a sample of C60 powder at a temperature of 450-1100°C.

Methodology Applied
Scientific EffectHeat treatment: Heat Treatment

Data Source

PatentUS12030777B2Method for preparing millimeter-sized sp<sup>3 </sup>amorphous carbon block material
Publication Date: 2024.07.09 JILIN UNIVERSITY
  • US12030777B2 patent drawing
  • US12030777B2 patent drawing
  • US12030777B2 patent drawing

AI summary

The invention relates to a millimeter-sized bulk spa amorphous carbon material and a method of preparing the same, and the method comprises a step of performing a high-temperature and high-pressure (HTHP) treatment on C60 powder at a temperature of 450-1100° C., preferably 700-1000° C., more preferably 900-1000° C., and most preferably 1000° C., and a pressure of 20-37 GPa, preferably 20-30 GPa, and most preferably 27 GPa, so as to obtain the millimeter-sized bulk sp3 amorphous carbon material. The sp3 carbon content in the amorphous carbon material is adjustable by changing the temperature and pressure conditions, so that the sp3 content is greater than 80%, and the sp3 content of high-quality samples is close to 100%. The optical band gap and thermal conductivity of the series of amorphous carbon materials can be effectively adjusted. The obtained series of amorphous carbon materials have ultra-high hardnesses, high thermal conductivities, adjustable band gaps (1.90-2.79 eV) which exceed the ranges of the band gaps of amorphous silicon and germanium. As a result, a new space is opened up for the application of amorphous materials.