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High infra-red blocking cellulose film based on amorphous to anatase transition of TiO via atomic layer deposition 2

Wenbin Li, Linfeng Li, Xi Wu, Junyu Li, Lang Jiang, Hongjun Yang, Guizhen Ke, Genyang Cao, Bo Deng, and Weilin Xu ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b03641 • Publication Date (Web): 09 May 2018 Downloaded from http://pubs.acs.org on May 9, 2018

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ACS Applied Materials & Interfaces

High infra-red blocking cellulose film based on amorphous to anatase transition of TiO2 via atomic layer deposition Wenbin Li,a† Linfeng Li,a† Xi Wu,a Junyu Li,a Lang Jiang,ab Hongjun Yang,ab Guizhen Ke,a Genyang Cao,a Bo Deng,*ab and Weilin Xu*a a

State Key Laboratory of New Textile Materials & Advanced Processing Technologies,

Wuhan Textile University, Wuhan, Hubei 430200, China. b

School of Material Science and Engineering, Wuhan Textile University, Wuhan, Hubei

430200, China. KEYWORDS: Infra-red blocking, Heat-insulated, Cellulose film, Crystal transition, Atomic layer deposition

Abstract A high IR-blocking cellulose film was designed based on an amorphous to anatase transition of TiO2 using atomic layer deposition(ALD). This transition was realized at 250 o

C, at which the cellulose is thermal stable. Optimized ALD condition of 250 oC and 1200

cycles give us an excellent heat insulator which could significantly reduce the enclosed space temperature from 59.2 oC to 51.9 oC after exposed to IR lamp for 5 min.

ACS Paragon Plus Environment

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Sharply increased energy consumption and subsequently boomed CO2 emission have been widely accepted as the major reason for the ocean acidification and climate warming.1 Before the wide application of a reliable green energy, energy conservation is the only option to alleviate above-mentioned environmental problems. Heat insulator are generally used as the outer coating of building which can efficiently reduce the energy consumption in daily life by slowing down the heat exchange between building and atmosphere particularly in hot summer and cold winter.2-5 High reflective index of TiO2 make it an excellent candidate for the fabrication of heat insulator with high IR-blocking properties.6-8 Thus, coating nano-scaled TiO2 onto cellulose film via sub-nanometric precise atom layer deposition (ALD) is attractive in the fabrication of new heat insulator by blocking the dominate infrared light in natural sunshine. Even though lots of works have been reported on the improvement of substance’s heat insulating property by TiO2 coating. Few reports are available for the driving of transformation from amorphous TiO2 to anatase TiO2, which is proved to be more IR-reflective than the former.9 In this letter, precisely tuned ALD parameters such as the cycle numbers and ALD temperatures implement the transition from an amorphous to anatase TiO2 coating, which efficiently enhances the heat insulating property of coated cellulose films. The ALD TiO2 was performed inside a home-made ALD reactor. Detailed reaction mechanism are shown in scheme 1.


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Typically, affluent surface-bounded -OH of cellulose film subsequently reacted with firstly introduced Titanium(IV) isopropoxide (TTIP) and secondly introduced water to form a chemically bonded monolayer of TiO2. By repeating abovementioned cycle to certain numbers, similar 2D-mode TiO2 layers with desired thickness are obtained.10 Temperature and cycle numbers are reported as two key parameters controlling the structure and properties of formed inorganic coating on various substrates.11-15 Particularly for the ALD TiO2, temperature is tightly linked with its transition from amorphous phase to crystal phase.16-19 Currently results reveal that a minimum temperature of around 500 oC is necessary for this transition.20,21 While most polymers are thermal-labile at this high temperature. Realization of this transition at low temperature which could survive the conventional polymers are highly desired for the functional polymer films via ALD TiO2. Thermal stable cellulose film up to 300 oC

(Figure S1) is used as a platform to perform ALD of TiO2 at various

temperature and cycle numbers (as shown in Table S1). Successfully coating of TiO2 onto cellulose film is proved by both attenuated total reflection-Fourier transform infrared (ATR-FTIR) and X-ray photo electron spectroscopy (XPS). For ATR-FTIR, the attenuation of peaks around 1060 cm-1 (COH stretching) and 1163 cm-1 (C-O-C vibration) with simultaneous blue-shift of peak from 1642 cm-1 (C=O) to 1632 cm-1 (Ti-O-C) after TiO2 coating prove both the existence of TiO2 coating and the chemical bonding between TiO2 coating and cellulose films (Table S2 and Figure S2). C1200T250 shows higher reflectance and lower transmittance than control sample to infrared at wavelength of 850-2000cm-1


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(Figure S2(b-c)), which provides an evidence that TiO2 coated films have better infrared blocking ability. Additional characteristic signals around 458 eV and 464 eV in the survey XPS of TiO2 coated cellulose film（Figure 1b）further indicates the existence of Ti. Clearly Ti 2p1/2 and Ti 2p3/2 peaks with a binding energy gap of

5.7 eV between

464.98 and 459.28 peaks is in good agreement with as

reported.22-24 Higher atomic ratio of 8:3 (O:Ti) than theoretical value of 2:1 according to the formula of TiO2. This abnormal ratio may implies a different coordination number and lattice arrangement of TiO2 in our case. Increased roughness of the surface of TiO2 coated cellulose films (Figure S3) along with accumulated ALD cycle numbers could be furtherly improved by AFM tests (Figure S4).

The RMS of coated

cellulose films as a function of cycle numbers of ALD at 250 oC (Figure S4e) clearly reveals this tendency. It was reported that coarsening by coalescence

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during the transformation from nano-sized amorphous TiO2 to anatase might be an important reason for the increasing in surface roughness. The significantly improved thermal stability of cellulose film after TiO2 coating is conformed by the higher residual weight percentage of all Cm-Tn films (m,n indicates cycle numbers and temperatures used in our ALD experiments, see Table S1) (Figure S1). It was reported that the anatase TiO2 normally reveal much higher blocking effect against infrared lights than amorphous TiO2.9 While the transition of amorphous TiO2 to anatase TiO2 is observed only when the temperature is higher than 500 o

C.20,21 At which most conventional polymer are thermal-labile. In our experiment,


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an obvious amorphous to anatase transition (Figure 2) was observed at 250 oC after 1200 cycles. Corresponding grain size of anatase TiO2 calculated based on Scherrer equation26 (as shown below) is 33.7 ±0.9 nm. d=

kλ β cos θ

Where d is the particle diameter, k is the Scherrer constant, a value of 0.89 was taken in this article; λ is the x-ray wavelength, a value of 0.15418nm was taken in this article; θ is the Bragg angle; β is the FWHM of a diffraction peak. One p-type silicon wafer (1×1 cm) together with each cellulose film were treated at different ALD conditions. Disappearing of significantly Si(400) peak around 69.14o in XRD of all Si wafers after ALD TiO2 further convinced that their surfaces were fully covered by TiO2.26 While different with the XRD of cellulose films after ALD, hardly could we see the signals of anatase TiO2 identified by 2θ of 25.28o, 37.80o, 48.05o, 55.06o,62.69o and 70.31o for (101), (004), (200), (211), (204), and (220) planes

26,27

respectively in Si-wafer treated same with C1200T250. This may

due to the much lower peak height of anatase TiO2 than Si (400). 28 It is obvious that 250oC are the lowest temperature which is possible to drive the phase transition of TiO2 from amorphous to anatase in our case. Besides, 800 cycles at 250oC is not sufficient for the amorphous to anatase transition of TiO2. Only after 1200 ALD cycles could we see clearly the anatase signals which implied longer crystal growth period are needed for the phase transition of TiO2 from amorphous to anatase.


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To further investigate the regulating effects of ALD parameters on the heat insulating property of TiO2 coated cellulose films, home-made apparatus as shown in Figure S4 was utilized. Blocking efficiency of TiO2 coated films are calculated according to the equation as shown below. WP =

×100%

Where WP is the blocking efficiency against infrared power, P0 is the IR power inside the case without installing cellulose films , P is the IR power inside the case after protected by TiO2 coated cellulose films. As shown in Figure 3(a), almost linear relationship between blocking efficiency and ALD cycle numbers before 400 cycles maybe ascribed to the property of amorphous TiO2. Matched linear relationship between residual weight and cycle numbers span the same cycle region in TGA (insert in figure S1) reveals the structure difference of TiO2 formed before and after 400 cycles at 250oC. Slowed increase in blocking efficiency with 800 and 1200 cycles at 250 oC is also in accord with the tendency of the residue weight along with temperature in TGA (Figure S1(a)). All these indicate that the phase structure and density of TiO2 both dominates the heat insulating properties of TiO2 coated films. The reduced thermaldecomposition rate of TiO2 coated cellulose films with increase ALD cycles also proved the thermal-stability enhancement of TiO2 to cellulose films which is similar as reported.8, 29 Significantly increased IR blocking efficiency of cellulose film from 10.6% (control) to 55.6% (C1200T250) also convinced the excellent heat insulating property of TiO2-coated cellulose film. To clarify the actual heat insulating effect of TiO2 coated cellulose films, space temperatures covered by TiO2 coated cellulose film (after various ALD cycles and


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temperatures) are measured by a thermal sensor as shown in Figure 3(b). TiO2 coated cellulose film (C1200T250) reveals best insulating property by reducing temperature from 32.5 oC to 28.6 oC among all films. IR-blocking effect of films as a function of infrared-light-irradiation time till 5 min was listed in Figure 3(c). Even after 5 min infrared light irradiation, the temperature under TiO2 coated cellulose film (C1200T250) is 7.3 oC lower than that under cellulose film. In conclusion, an amorphous to anatase phase transition of TiO2 could be driven at a ALD temperature of 250oC after 1200 cycles. The low transition temperature (starting decomposition temperature of cellulose is ~300 oC) could survive cellulose films which finally generate an excellent heat insulator. This new material are very promising to act as an new building heat insulator which could efficiently alleviate energy consumption and subsequently boomed carbon emission.

ASSOCIATED CONTENT Supporting Information. The Supporting Information is available free of charge on the ACS Publications website. Thermogravimetric analysis of TiO2 coated cellulose films treated at different ALD cycles, denotation of samples treated by ALD TiO2 at different cycles and temperatures, representative ATR-FTIR spectra of cellulose films before and after ALD including the attributions of different FTIR peaks, XPS survey spectra of the cellulose films treated by ALD TiO2 at different cycles and temperatures, XPS spectra of the Ti2p peaks of the cellulose films treated by ALD TiO2 at different cycles and temperatures, SEM surface


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morphology of cellulose films, and device used to evaluate the heat insulating properties of TiO2 coated cellulose films.

AUTHOR INFORMATION Corresponding Author *Bo Deng:[email protected] *Weilin Xu: [email protected] Author Contributions The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript. †Wenbin Li and Linfeng Li contributed equally. Notes The authors declare no competing financial interest.

ACKNOWLEDGMENT This research was financial supported from the National Key R&D Program of China (Grant No. 2017YFB0309100) and the National Natural Science Foundation of China (Grant No. 51773158), National Science Foundation for Distinguished Young Scholars (Grant No. 51325306) . The authors would like to acknowledge the Key Laboratory of Textile Fiber & Product (Wuhan Textile University) Grant (Project no. FZXW2017013) for support of this project.

REFERENCES


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SCHEMES

Scheme 1. Reaction mechanism of ALD TiO2 onto cellulose film.


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FIGURES

Figure 1. (a) XPS survey spectra of the cellulose films treated by ALD TiO2 at different cycles and temperatures.; (b) XPS spectra of the Ti 2p peaks of the cellulose films treated by ALD TiO2 at different cycles and temperatures.


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Figure 2. (a) XRD of silicon wafers treated by various ALD cycles and temperature and (b) XRD of cellulose films treated with various ALD cycles and temperature.


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Figure 3. (a) Blocking efficiency of cellulose films against infrared light with various ALD cycles and temperatures and (b) space temperature under TiO2 coated cellulose films with various ALD cycles and ALD reaction temperature; (c) space temperature under control and C1200T250 films with infrared light illuminating time.


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