1. Introduction

2. Creating Cellulose Aerogel

Table 1. Classification of Cellulose-based aerogel together with published examples from.

3. Characterization Methods of Cellulose-Based Aerogels

3.1. Characterization of Cellulose Aerogels’ Structure

By applying the structural characterization to the cellulose aerogels, it can be answered that rigidness, or flexibility, physical properties of material, containing the component type such as organic or inorganic or how small or large porous it has [115].

The essential structural parameters of a porous material include the overall fraction of the pore and solid phase, the typical size of the backbone and pore phase, the connectivity between two phases, properties of interface between them, and the molecular structure of the backbone phase. These characteristics are evaluated using various characterization methodologies [115].

3.1.1. Microscopic Analyses

Microscopy techniques offer valuable visual insights into the structure of aerogels at various length scales, including those as small as a few Angstroms. While light microscopy (LS) has a resolution boundary of around 500 nm, it fails to capture the properties of most aerogels due to their particle sizes typically less than 1 mm. Atomic force microscopy (AFM) theoretically has the potential to be used for aerogels but proves to be challenging in practice due to the irregular and deep surface topology found in fractured aerogels [115].

Consequently, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) are the primary microscopic techniques employed in aerogel research. SEM allows for the visualization of the three-dimensional interconnected structure of the aerogel backbone, with a maximum resolution of approximately one nanometer. In contrast, TEM has better resolution capabilities and can examine the substructure of the particles that make up backbone as well as any other phases employed into the aerogel skeleton, like metal particles. The released electrons and X-rays inside the hemisphere of main beam are examined using a reflection setup in SEM mode. TEM, in contrast, investigates the sample’s transmission by high-energy primary electrons. All high-resolution electron microscopes operate with a chamber vacuum of less than 10^-4 mbar to reduce undesired scattering [115].

Figure 3. SEM images of various cotton samples: a) untreated cotton, b) cotton loaded with TA, c) cotton loaded with TA/B, and d) cotton coated with TA/B@PDA. The images were taken at different magnifications, specifically a) 100, a1) 2000, and a3) 5000 respectively (The permission is approved by the John Wiley and Sons, Macromolecular Materials & Engineering under License number:5570770529195) [116].

Figure 3. SEM images of various cotton samples: a) untreated cotton, b) cotton loaded with TA, c) cotton loaded with TA/B, and d) cotton coated with TA/B@PDA. The images were taken at different magnifications, specifically a) 100, a1) 2000, and a3) 5000 respectively (The permission is approved by the John Wiley and Sons, Macromolecular Materials & Engineering under License number:5570770529195) [116].

3.1.2. Scattering Techniques

Scattering techniques provide a quantitative and noninvasive means of analyzing the structure, without causing damage to the sample [117]. Moreover, it proves to be a valuable technique for assessing the transparency of aerogels, investigating their pore size, structure, and mechanical strain, as well as exploring the sol-gel evolution modes that shape their microstructure. The examination of wavelength-dependent scattering enabled by ultraviolet-visible transmission spectroscopy permits comparisons across aerogels of various sources and thicknesses, as well as analyzing the influence of residual pollutants. Infrared reflectance tests provide the actual real and hypothetical refractive indices of porous aerogel materials, allowing researchers to better understand material characteristics and radiant heat transport. Scattering measurements at a given angle are useful for quality control, locating scattering sources, and evaluating inhomogeneities [118].

The dispersed intensity of aerogels often displays radial symmetry, suggesting an isotropic material. As a result, in a certain experimental arrangement, the angle θ becomes the only variable. However, if the aerogel sample has anisotropic qualities (due to drying conditions, for example), anisotropy will be seen in the scattering pattern, necessitating the use of directional information to explain the orientation of the anisotropy. In general, scattering is classified into two types: small-angle scattering (SAS) and wide-angle scattering (WAS). When employing a reflection setup, X-ray scattering is often referred to as X-ray diffraction (XRD). SAS employs scattering angles (2θ) ranging from 0.001° to nearly 10°, with wavelengths between a few angstroms and nanometers. The equivalent q-range is 5 to 10^-4 nm^-1, with the lowest q limit observed in ultra-low-angle scattering (USAXS and USANS) [118,119,120].

3.1.3. Thermoporometry

Cellulosic aerogels’ outstanding capabilities are greatly influenced by their hierarchical pore structure. However, utilizing a single approach for examining the complete pore size distribution (PSD) might be difficult. Mercury infiltration and nitrogen sorption are the most often used techniques for evaluating the PSD of aerogels. Nitrogen sorption, on the other hand, only protects pores up to around 170 nm, which is insufficient for the vast PSDs observed in cellulosic aerogels that span the single-digit nanometer to low micrometer range. On the other hand, mercury intrusion is not suitable for characterizing fragile and ultra-lightweight cellulose aerogels as it tends to destroy the delicate nanofibrillar network of these soft materials. As a result, estimating the bulk volume decrease (sample compression) instead of monitoring mercury penetration into the pore network (non-intrusive mercury porosimetry) is the only way to calculate the PSD. Nitrogen sorption tests can be used to characterize the PSD under the greatest pore size impacted by densification after applying a given mercury pressure [121,122]. Thermoporometry is a technique that examines the freezing behavior of a liquid within pores. By analyzing the resulting data, it is possible to extract details regarding the arrangement of pore sizes and the morphology of the pores. This technique is particularly sensitive to pores within the range of 2 to 30 nm. Unlike traditional porosimetry methods that involve mercury or gas adsorption and require dry samples, thermoporometry can be applied to gels, eliminating the need for sample drying [115]. It is a proposed method that offers a different approach to characterizing the structure of porous aerogels. It depends on the utilization of the Gibbs-Thomson equation, which was introduced by Gibbs in 1928 and Thomson in 1872. This equation measures the experimental shift in an interstitial liquid’s melting point caused by confinement within microscopic pores [123,124].

3.1.4. Gas Sorption

The processed macro-meso porous aerogels displayed the following characteristics concerning the flow of air passing through them in the atmosphere:

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Pressure-time curves were consistent with that of theoretical model created for pure Darcy flow, which was employed to fitting the data and get the permeability constant.

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Permeability remained consistent regardless of the difference in pressure.

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Choice of surfactant had an impact on the permeability.

Above mentioned findings display that Darcy’s law may be used without considering other effects such as Knudsen effects, Klinkenberg effect or slip flow at cell walls [125,126,127]. The commonly employed method for characterizing aerogels is nitrogen (N₂) sorption at a temperature of 77.3 K. An extensive variety of relative gas pressures, ranging from 0 to 1, may be obtained by adjusting the gas pressure from vacuum to 0.1 MPa (1 bar). This method often yields useful data on particular surface areas as low as 0.01 m²/g and pore diameters ranging from 0.3 to 100 nm [115].

3.1.5. Hg Porosimetry

Porosimetry using mercury (Hg) is a technique capable of investigating a broad range of accessible pore sizes, spanning approximately six orders of magnitude. This range extends from about 400 mm down to a few Angstroms [128]. In theory, Hg porosimetry may be used to examine the distributions of pore sizes spanning between microns and nanometers. On the other hand, when working with flexible materials like aerogels, considerable deformation effects may arise unless the sample stiffness aligns well with the pore size [129,130]. One drawback of mercury porosimetry is that it frequently leads to irreversible deformation of the sample, and a portion of infiltrated mercury becomes captured. Consequently, the sample is rendered unusable for subsequent investigations and must be disposed of as toxic waste [115]. Consequently, a comparative study on pore size measurement of cellulose-based aerogels revealed no observable damage or degradation in the aerogel produced from softwood pulp cellulose nanofibrils [131].

3.2. Mechanical Characterization of Cellulose Aerogels

Thorough mechanical characterizations are essential in assessing the suitability of aerogels for load-bearing applications, as it is crucial to understand their mechanical response under operational conditions. Mechanical characterization studies must be meticulously constructed to reproduce or nearly match the loading conditions met in the desired service environment. Since aerogels can be subjected to diverse service conditions, it is necessary to perform multiple types of loading tests to fully evaluate their mechanical response. These tests generally encompass compression, bending, tension, multiaxial stress states, and torsion under various loading circumstances such as dynamic, fatigue and quasi-static. Following approaches are routinely used in this regard [132].

3.2.1. Differential Scanning Calorimetry (DSC), Dynamic Mechanical Analysis (DMA)

DSC is a technique for measuring thermal effects during heating of materials (e.g. glass transition temperature). The relationship between the rigidity of aerogels and temperature is determined using DMA. DMA uses alternating loads at a constant frequency, generally 1 Hz, or changing frequencies ranging from 0.1 to 20 Hz. The tests are carried out at temperatures ranging from -100 °C to 300 °C, with the setup for a three-point bending test. Dynamic Mechanical Analysis (DMA) findings display the loss and storage moduli as they vary with temperature. The peaks observed in the loss tangent as a function of temperature can serve as indicators for identifying the glass transition temperatures [133].

3.2.2. Tension, Compression

Aerogels are not well-suited for conducting impact tests, hence the approach used to quantify strength may be problematic from an engineering standpoint. Bending or tensile testing are preferable. The test should be tailored to the material [134]. Furthermore, determination of the compressive stiffness of aerogel composites by microstructure’s effectiveness in transmitting applied stress and is regulated by the solid content. The density of the composite increases with higher solid content, resulting in higher stiffness [135]. Aerogel elastic characteristics are commonly assessed using sound velocity measurements [136,137,138] or static methods [139,140,141,142]. It is well accepted that silica and cellulosic aerogels are "fragile materials" because of the low mechanical properties caused by the network’s limited connectivity and large porosity. The existence of defects, which act as stress concentrators, has a significant impact on rupture resistance [141,142,143,144,145,146]. Dog-bone-shaped specimens (as per ASTM D638) are often used for tension testing. Similarly, compression testing may be performed on cylindrical specimens (following ASTM D695). It is critical to prepare the specimen surfaces so that they are smooth and free of flaws. The end surfaces of cylindrical compression specimens should be parallel to one other. To avoid mistakes, compression tests should be done on compression plates with extremely parallel surfaces, especially for brittle aerogels. To achieve adequate alignment, a frequently employed method is the utilization of a self-aligned compression fixture. It is necessary to calculate the entire stress-strain relationship, including the point of ultimate failure, at exceedingly low strain rates to evaluate the energy absorption capacity and strength, as represented by area under stress-strain curve. To assess the dimensional stability of samples, conducting constant deflection-compression set tests (referred to as Test-D in ASTM D3574 Standard) is feasible. This test involves measuring the changes in thickness of cylindrical specimens exposed to a range of compression strains at an elevated temperature for a specified duration [115].

3.2.3. Sound Absorption and spreading

Noise pollution, considered the second most significant environmental hazard impacting human well-being and living conditions after air pollution, necessitates the utilization of porous sound absorption materials. These materials offer remarkable attributes like a broad range of sound absorption frequencies, cost-effectiveness, and ease of shaping. With its voluminous porous structure characterized by low density, high porosity, and extensive surface area, aerogel allows acoustic waves to enter deeply into its structure, enabling diverse interactions to occur [147,148,149,150].

Acoustic performance evaluations are often performed using an impedance tube (SW422, SW477, BSWA Technology Co. Ltd., China) in accordance with ASTM E1050-10 [151]. Sound absorption coefficient is expressed as α= (E_i - E_r)/E_i, where E_i denotes incoming acoustic energy and E_r denotes reflected acoustic energy. For sound absorption testing, samples having diameters (100 mm and 30 mm) are used, with frequency in the ranges of 200-1000 Hz and 1000-6300 Hz, respectively [152,153,154]. A demonstration was also carried out to evaluate the sound insulation capabilities of silica-cellulose aerogels and their cellulose matrices. The experiment used a sound signal generator (Blesi Guardian angel anti-rape alert, 90 dB) to generate known sound signals with a specified sound strength. The coefficient of absorption of sound for the silica-cellulose aerogels and the cellulose matrices was measured using a sound meter (Amprobe SM-10, USA). The sound generator was positioned both inside and outside of an insulating box. The insulating box was built by taping a certain type of aerogel to both sides of the container, resulting in a sealed system. In all situations, the incident sound signal was measured at an equidistant position from the sound generator. The absorbed sound intensity was determined by subtracting the known sound intensity from the incident sound intensity. The coefficient for sound absorption was computed as the ratio of absorbed sound intensity to known sound intensity [155].

Figure 4. The schematic picture depicts the principle of measurement of sound absorption coefficient with an impedance tube at several frequency ranges. The frequencies in Figure (a) vary from 50 to 1000 Hz, whereas the frequencies in Figure (b) extend from 500 to 6300 Hz [154] (Permission is granted by Creative Commons CC-BY license).

Figure 4. The schematic picture depicts the principle of measurement of sound absorption coefficient with an impedance tube at several frequency ranges. The frequencies in Figure (a) vary from 50 to 1000 Hz, whereas the frequencies in Figure (b) extend from 500 to 6300 Hz [154] (Permission is granted by Creative Commons CC-BY license).

4. Properties of Cellulose Aerogels

Table 2. Summarizing Characteristics of Cellulose-Based Aerogels.

5. Multifunctional Application of Cellulose-Based Aerogels on Textile Structures

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Other components can be added to the cellulose solution/suspension [11]. For example, the reaction of CNF with N-methylol-dimethyphospylpropionamide (MDPA) and further cross-linking by 1,2,3,4-butane tracarboxylic acid (BTCA) yields a flame retardant with good flexibility and self-extinguishment [180].

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Coating or adding additional substances to the aerogel structure [11], such as the polyacrylonitrile-silica aerogel coating over viscose nonwoven fabric for protection and comfort [181]. Another area of study is the application of molecular layer by layer (m-LBL) technology. This technique enables the deposition of ultra-thin layers onto a surface through sequential covalent processes. As a consequence, a precise molecular-scale coating is generated, mostly by surface oligomerization, which is not possible with bulk synthesis techniques [182,183,184].

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Surface modification of cellulose aerogels may be attained using a number of methods [11], including dip-coating with PDMS (Poly(dimethyl siloxane)) [185].

5.1. Thermal Insulation Materials

Materials are classified according to their thermal conductivity as thermal conductors (λ_eff ≥0.1W/(mK), insulators (0.1 W/(mK)>λ_eff >0.025 W/(mK), and super-insulators (λ_eff ≤0.025 W(mK). It is known that thermal conductivity of dry air is around 0.025 W/(mK), generally slightly dependent on temperature and moisture content.

Due to their thermal conductivity levels spanning from tens to hundreds of W/(mK), metals are good thermal conductors. Expanded polystyrene, extruded polystyrene, glass wool, mineral wool, and wood exhibit thermal conductivities within the range of 0.1 to 0.026 W/(mK), making them effective insulators against heat transfer [158,188]. Silica aerogels, vacuum insulation panels and vacuum glasses are regarded as super insulating materials as their thermal conductivity is below 0.025 W/(mK) [189].

The thermal conduction of aerogel can be classified as solid-state, gas-phase, open-pore, or radiation thermal conduction. Once the pore size of a porous material approaches the average free path of the gas (which is approximately 70 nm when vented), the thermal conductivity of the substance decreases. This is attributed to the fact that the pores impede gas flow and restrict convection, thereby hindering heat transfer. The thermal conductivity of mesoporous cellulose aerogels primarily depends on two factors: solid-state thermal conduction and gas-phase thermal conduction. These factors, in turn, are closely associated with the aerogel density (determined by the initial cellulose concentration), the distribution of pore sizes, and the surface structures of the aerogel material [11].

Regenerated cellulose aerogels possess a porous structure with a relatively higher fraction of large pores compared to other cellulose aerogels. This increased presence of large holes within the aerogel structure enhances heat conductivity as it facilitates improved gas transport [11].

Antlauf et al. conducted a study in which cellulose fibers (CFs) and cellulose nanofibers (CNFs) were produced from commercially available birch pulp. The production process involved varying pressure and temperature parameters as experimental variables. For temperatures ranging from 80 to 380 °C, their results exhibited very little fluctuation in thermal conductivity with density (ρ_sample = 1340-1560 kg/m^-3). Furthermore, temperature dependency is independent of fiber size, density, and porosity.

Figure 5 depicts their studies on thermal conductivity [190]. Thai et all studied the oil repellency and insulation properties with the sugarcane fiber by sol-gel synthesis and using freeze-drying. According to their findings, increasing sugarcane fiber content has a substantial influence on thermal conductivity ranging between 0.031 and 0.042 W/(mK) [191].

Table 3. Thermal insulation properties and application of cellulose-based aerogels.

Table 3. Thermal insulation properties and application of cellulose-based aerogels.

No.	Material	Drying Method	Thermal Conductivity	Pore Size	Density	Application	Reference
1	Raw pineapple-leave fibers (PALF)	Freeze-drying	0.030-0.034 W/mK	1.38nm-2.21 nm	0.04 g/cm3	Heat and sound app.	[72]
2	Aerogels composed of bidirectional anisotropic polyimide/bacterial cellulose (b-PI/BC)	Freeze-drying	23 mW/mK- 44 mW/mK (bidirectional PI/BC aerogels) 37 mW/mK -66 mK/mK (unidirectional PI/BC aerogels)	10–20 μm	46 mg/cm3	Practical and complex thermal insulation applications in buildings and aerospace	[192]
3	Aerogels made of fibrous silica and bacterial cellulose (BC)	Ambient pressure drying	-	13.7-15.5 nm	0.164 g/cm3	Wearable substances	[193]
4	Holocellulose nanofibrils/cellulose aerogel fiber (HCAFs)	ScCO2 drying	0.048 W/mK	265.4 ± 34.5 nm	0.22 g/cm3	Wearable substances	[163]
5	Multiscale nanocelluloses (NCs)	Freeze-drying	25.4 mW/mK	32 - 48 nm	7.2 kg/m3	Thermal insulation app.	[194]
6	Textile waste fibers (TWF) aerogel	Freeze-drying	0.049 - 0.061 W/mK	-	0.040-0.096 g/cm3	Building insulation and oil spill cleanup.	[195]
7	Nanofibrous Kevlar Aerogel Threads	ScCO2 drying and Freeze-drying	0.036 W/mK	11-12.8 nm	13 g/cm3	Thermal insulation and thermal management.	[196]
8	Hydrophilic recycled cellulose aerogels	Freeze-drying	0.029 -0.032 W/mK	40-200 µm	0.040 g/cm3	Sorption of water/oil, resistance of water, and thermal insulation	[197]
9	Silk fibroin aerogel	Freeze-drying	0.031 W/(mK)	19.71 ± 8.53	0.21 g/cm3	High performance thermal insulation	[198]
10	Aerogels made of nanofibrillated cellulose	Spray lyophilization	0.018 W/(mK)	10 to 100 nm	0.012–0.033 g/cm3	Thermal super insulating material	[110]

6. Companies of Producing Cellulose Aerogels

7. Global Market Study Focused on Cellulose-based Aerogel and Their Future Aspects

8. Conclusion

9. List of Abbreviations

Declaration of Competing Interest

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