CN114316376B - CNF/BNNS composite dispersion liquid, film and preparation method - Google Patents
CNF/BNNS composite dispersion liquid, film and preparation method Download PDFInfo
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Abstract
The invention discloses a CNF/BNNS composite dispersion liquid, a film and a preparation method thereof, which comprises the following steps: carrying out TEMPO oxidation on a suspension of macroscopic cellulose fiber slurry, adjusting the pH of the suspension to be alkaline, adding absolute ethyl alcohol for quenching after oxidation, carrying out suction filtration, and adding water into an obtained filter cake for dispersion to obtain a first dispersion liquid; adding boron nitride powder into the first dispersion liquid to obtain a second dispersion liquid, and performing ball milling to obtain a third dispersion liquid; and (4) carrying out ultrasonic treatment on the third dispersion liquid, and homogenizing to obtain the CNF/BNNS composite dispersion liquid. The composite dispersion liquid has good dispersibility and stability, and a composite film prepared from the composite dispersion liquid has good heat conductivity and mechanical properties, and can be used for packaging electronic equipment.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a CNF/BNNS composite dispersion liquid, a CNF/BNNS composite dispersion film and a preparation method thereof.
Background
With the rapid development of electronic devices toward miniaturization and high power, the heat dissipation problem becomes increasingly urgent as the large amount of heat generated by the devices inevitably results in thermal failure, reduced performance, and shortened service life. At present, polymer matrix composite materials are widely used as thermal management materials in the field of electronic devices due to the advantages of excellent processability, good flexibility, low cost and the like.
Hexagonal boron nitride (h-BN) as a thermally conductive filler having excellent heat transfer properties (400 W.m) -1 K -1 ) Structural stability and oxidation resistance. Boron Nitride Nanosheets (BNNS) obtained by bulk h-BN stripping due to reduced number of layersThe interlayer interaction and coupling deviate from the two-dimensional selection rule, so that phonon-phonon scattering is reduced, and the bulk h-BN has higher thermal conductivity (600 W.m) -1 K -1 ). Furthermore, BNNS is more favorable for forming a heat conducting network in the polymer due to its smaller thickness. Thus, BNNS is more suitable as a thermally conductive filler for polymer matrices than bulk h-BN. At present, there are two main strategies for BNNS production: one is to grow BNNS from bottom to top by a chemical vapor deposition method, which can only deposit a small amount of film and is difficult to produce in volume; another strategy is to peel the bulk h-BN into a nano-lamellar structure from top to bottom by mechanical or chemical methods. Common methods of exfoliation are: the method comprises the steps of molten alkali etching, ultrasonic stripping, hydroxide-assisted ball milling stripping, air oxidation stripping and the like, and the stripping method is relatively simple and feasible and is expected to realize large-scale production. However, these current stripping methods suffer from drawbacks, either in low yield or high cost, and the h-BN is cleaved during the stripping process, resulting in the production of BNNS with small lateral dimensions.
It is well known that the addition of thermally conductive fillers to polymers can improve the thermal conductivity of the polymer matrix, but achieving uniform dispersion of the filler in the polymer matrix is a very challenging task. For BNNS, it is difficult to disperse uniformly in a polymer matrix, especially at higher addition levels, due to the high surface energy of the nanomaterials themselves and the strong van der waals interactions and chemically inert surfaces between BNNS. Effective dispersion of the thermally conductive filler is a fundamental requirement for thermally conductive composites to improve the thermal conductivity of the polymer matrix, since a contacting network of thermally conductive fillers interconnected is required to create an optimal thermal conduction path through the matrix via filler-to-filler communication.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a CNF/BNNS composite dispersion liquid, a film and a preparation method thereof, TEMPO oxidized cellulose fibers and boron nitride are mixed and ball-milled, and then the cellulose nanofiber/boron nitride nanosheet (CNF/BNNS) composite dispersion liquid is prepared through high-pressure homogenization treatment, the dispersion liquid has good dispersibility and stability, and the composite film prepared by the dispersion liquid has good heat conductivity and mechanical properties and can be used for packaging electronic equipment.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of CNF/BNNS composite dispersion liquid comprises the following specific steps:
s1, TEMPO oxidation is carried out on suspension of macroscopic cellulose fiber slurry, the pH value of the suspension is adjusted to be alkaline, absolute ethyl alcohol is added after oxidation to be quenched and filtered, and water is added into an obtained filter cake to be dispersed to obtain first dispersion liquid;
s2, adding boron nitride powder into the first dispersion liquid to obtain a second dispersion liquid, and performing ball milling to obtain a third dispersion liquid;
and S3, carrying out ultrasonic treatment on the third dispersion liquid, and homogenizing to obtain the CNF/BNNS composite dispersion liquid.
Further, in step S1, the content of cellulose fibers in the suspension of the macroscopic cellulose fiber slurry is 0.5wt.% to 1.5wt.%.
Further, in step S1, adding 0.01-0.03 g of TEMPO, 0.1-0.3 g of NaBr and 2-5 mmol of NaClO to the suspension in sequence to carry out TEMPO oxidation.
Further, in step S2, 0.1 mol. L is used -1 ～0.2mol·L -1 Adjusting the pH value of the NaOH solution to 9-11, oxidizing for 2-4 h, adding 2-5 mL of absolute ethyl alcohol for quenching, and keeping the pH value of the mixed solution at 9-11 during oxidation.
Further, in step S2, the amount of boron nitride added to the second dispersion is 10wt.% to 50wt.%.
Furthermore, in the step S2, ball milling is carried out for 9-15 h under the conditions that the ball mass ratio is (1-1.5): 1 and the rotation speed of the ball mill is 400-600 rpm.
Further, in the step S3, the ultrasound is performed for 2 to 4 hours under the condition of 500 to 700W; the homogenization is to carry out homogenization treatment for 20 to 40 times under the condition of 50 to 100 MPa.
Further, in step S1, the macroscopic cellulose fiber slurry is a slurry made of wood, seed fiber, bast fiber or grass.
The invention also providesThe CNF/BNNS composite dispersion liquid prepared by the preparation method is used for preparing the CNF/BNNS high-thermal-conductivity film, and the thermal conductivity of the CNF/BNNS high-thermal-conductivity film is 0.103 W.m -1 K -1 ～0.188W·m -1 K -1 The strength is 30MPa to 60MPa, and the elongation at break is 2 percent to 5 percent.
Further, the preparation method of the CNF/BNNS high thermal conductive film comprises the following steps:
1) Diluting the CNF/BNNS composite dispersion liquid, and performing suction filtration to obtain a filter cake;
2) The obtained filter cake is subjected to cold pressing and drying to obtain the CNF/BNNS high-thermal-conductivity film;
the CNF/BNNS high thermal conductive film is used for packaging electronic equipment.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention discloses a preparation method of a nano-cellulose/boron nitride nanosheet (CNF/BNNS) composite dispersion liquid, which is characterized in that cellulose fibers subjected to TEMPO oxidation and bulk boron nitride are mixed and peeled, and the interaction between the cellulose fibers and the bulk boron nitride is enhanced while the cellulose fibers and the bulk boron nitride are peeled through a ball-milling and homogenizing two-step peeling process, so that the stable dispersion of BNNS is realized. In addition, the addition of cellulose and the homogenization process greatly promote the dispersion stability of BNNS.
The CNF/BNNS composite dispersion liquid prepared by the invention is uniform and stable, has good dispersibility, and the film prepared by using the CNF/BNNS composite dispersion liquid as the raw material has good mechanical property and thermal conductivity, and can be used for packaging electronic devices.
Furthermore, the raw material cellulose adopted by the invention has low price, wide source and biodegradability, and meets the requirement of environmental protection.
Drawings
FIG. 1 is an optical photograph of CNF, BNNS and CNF/BNNS dispersions obtained by different preparation processes;
FIG. 2 is an SEM photograph of a dispersion of example 4;
FIG. 3 is a TEM image of a dispersion of example 4;
FIG. 4 is a stress-strain diagram of a CNF/BNNS composite film prepared with a BN added in an amount of 0 to 50 wt.%;
FIG. 5 is a thermal conductivity diagram of CNF/BNNS composite films prepared under different BN addition amounts;
fig. 6 is a temperature reduction curve of a pure CNF film and a CNF/BNNS composite film with 30wt.% BN addition.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
The invention relates to a method for preparing cellulose nanofiber/boron nitride nanosheet (CNF/BNNS) composite dispersion liquid and film by a ball milling homogenization method, which comprises the following steps:
(1) Adding deionized water into the macroscopic cellulose fiber slurry, uniformly stirring, and defibering for 5min to obtain a suspension with the cellulose fiber content of 0.5-1.5 wt% for later use.
(2) Magnetically stirring the slurry after being defibered in the step (1), sequentially adding 0.01-0.03 g of TEMPO (2,2,6,6-tetramethylpiperidine-nitrogen-oxide), 0.1-0.3 g of sodium bromide (NaBr) and 2-5 mmol of sodium hypochlorite (NaClO), and adding 0.1-0.2 mol.L -1 Adjusting the pH value of a sodium hydroxide solution (NaOH) to 9-11, oxidizing at room temperature for 2-4 h (keeping the pH value at 9-11, adjusting the pH value once every 0.5 h), adding 2-5 mL of absolute ethyl alcohol to quench after the reaction is finished, performing vacuum filtration to remove a solvent, washing with deionized water to be neutral, adding water into the obtained filter cake to 200g, stirring and dispersing to obtain a first dispersion.
(3) And (3) weighing 0.17-1.5 g of boron nitride powder, adding the dispersion liquid prepared in the step (2), and uniformly stirring to obtain a second dispersion liquid with the boron nitride addition of 10-50 wt.%.
(4) And (3) ball-milling the dispersion liquid prepared in the step (3) for 9-15 h, wherein the ball-material mass ratio is (1-1.5): 1, and the rotating speed of the ball mill is 400-600 rpm to obtain a third dispersion liquid, and the ball-milling is simple, easy to operate and suitable for large-scale production.
(5) And (3) carrying out ultrasonic treatment on the third dispersion liquid at 500-700W for 2-4 h, and homogenizing for 20-40 times at 50-100 MPa to obtain the CNF/BNNS composite dispersion liquid. The diameter of CNF in the dispersion is 20-50 nm, the length is 1-2 μm, and the ultrasonic treatment is used for preventing the third dispersion from flocculating and influencing the subsequent homogenization effect; the higher the pressure at homogenization, the smaller the diameter and the larger the aspect ratio of the cellulose cleaved CNF, and the thinner the exfoliated BNNS sheet, but the smaller the lateral dimension.
Preferably, the macroscopic cellulose fiber pulp is a pulp made of wood (softwood and hardwood), seed fiber (cotton, coconut, etc.), bast fiber (flax, hemp, jute, ramie, etc.) or grass (bagasse, bamboo, etc.).
Preferably, the CNF/BNNS composite dispersion liquid can be used for preparing the CNF/BNNS high thermal conductivity film, and the thermal conductivity of the CNF/BNNS high thermal conductivity film is 0.103 W.m -1 K -1 ～0.188W·m -1 K -1 The strength reaches 30 MPa-60 MPa, the elongation at break reaches 2% -5%, and the composite material has good heat transfer performance and mechanical strength and can be used for packaging electronic equipment.
The specific preparation steps of the CNF/BNNS high thermal conductive film are as follows:
1) Weighing a CNF/BNNS composite dispersion liquid with the absolute dry mass of 50mg, adding deionized water to dilute to 1 mg.L -1 The CNF/BNNS composite film is assembled into a paper-based material through vacuum-assisted suction filtration, the obtained paper-based material filter cake is cold-pressed for 2-5 min under 20-40 MPa, and then is dried for 10-15 min under vacuum at 80-120 ℃ to obtain the uniform CNF/BNNS composite film.
Example 1:
(1) Weighing macroscopic cellulose fiber slurry containing 1.5g of oven-dry mass, adding deionized water to 150g, uniformly stirring, and defibering for 5min to obtain suspension containing 1wt.% of cellulose fiber for later use.
(2) Magnetically stirring the slurry after the defibering in (1), sequentially adding 0.024g TEMPO (2,2,6,6-tetramethylpiperidine-nitrogen-oxide), 0.15g sodium bromide (NaBr) and 2.5mmol sodium hypochlorite (NaClO), and adding 0.1 mol. L -1 Adjusting the pH value of sodium hydroxide (NaOH) to 10.5, oxidizing at room temperature for 3h (keeping the pH value at 10.5, adjusting the pH value once every 0.5 h), adding 3mL of absolute ethyl alcohol after the reaction is finished, quenching, performing vacuum filtration to remove the solvent, washing with deionized water to be neutral, adding water to 200g of filter cake, stirring and dispersing to obtain a first dispersion liquid.
(3) Weighing 1.5g of boron nitride powder, adding the dispersion liquid prepared in the step (2), and uniformly stirring to obtain a second dispersion liquid with the boron nitride addition of 50wt.%.
(4) And (3) ball-milling the dispersion liquid prepared in the step (3) for 12h, wherein the mass ratio of ball materials is 1.2.
(5) And (3) carrying out ultrasonic treatment on the third dispersion liquid at 600W for 2h, and homogenizing for 40 times under 60MPa to obtain the CNF/BNNS composite dispersion liquid. The diameter of CNF in the dispersion is 20-50 nm, the length is 1-2 μm, and the ultrasonic treatment is to prevent the third dispersion from flocculating and affecting the subsequent homogenization effect; the higher the pressure at homogenization, the smaller the diameter and the larger the aspect ratio of the cellulose cleaved CNF, and the thinner the exfoliated BNNS sheet, but the smaller the lateral dimension.
Example 2: this example differs from example 1 only in that: the amount of boron nitride added was 10wt.%.
Example 3: this example only differs from example 1 in that: the addition amount of boron nitride was 20wt.%.
Example 4: this example differs from example 1 only in that: the amount of boron nitride added was 30wt.%.
Example 5: this example differs from example 1 only in that: the amount of boron nitride added was 40wt.%.
FIG. 1 is an optical photograph of CNF, BNNS and CNF/BNNS dispersions obtained by different preparation processes. BNNS-I, BNNS-II, CNF-BNNS-III, CNF-BNNS-IV and CNF-BNNS-V represent the addition of BN in amounts of 10wt.%, 20wt.%, 30wt.%, 40wt.% and 50wt.%, respectively,
(a) Mixing TEMPO oxidized cellulose fiber and BN, ball-milling and stripping at 500rpm, then carrying out ultrasonic treatment for 2 hours, and centrifuging at 4000rpm for 10min to obtain supernatant; (b) Mixing TEMPO oxidized cellulose fiber and BN, ball-milling and stripping at 500rpm, then carrying out ultrasonic treatment for 2h, homogenizing for 40 times at 60MPa, and finally centrifuging at 4000rpm for 10min to obtain supernatant; it can be seen that after standing for 30 days, the cellulose-added and homogenized dispersion had no obvious sedimentation and was well dispersed, indicating that the stable dispersion of BNNS by the cellulose-added and homogenized treatment was deficient;
FIG. 2 is an SEM photograph of the dispersion of example 4. It can be seen that the composite dispersion prepared by this method has a CNF diameter of 20 to 50nm, a length of 1 to 2 μm, and a BNNS lateral dimension of about 300nm.
FIG. 3 is a TEM image of the dispersion of example 4. As can be seen, BNNS has a lateral dimension of about 200-500 nm.
Fig. 4 is a stress-strain diagram of the CNF/BNNS composite film prepared when the BN addition amount is 0 to 50wt.%. It can be seen that when the addition amount of BN is 10wt.% to 40wt.%, the strength of the obtained composite film is greater than 50MPa, the elongation at break is about 4%, and the composite film has good mechanical strength, and when the addition amount of BN is 50wt.%, the strength and the elongation at break are reduced to a certain extent, and the strength of the obtained composite film can still reach 37MPa, and the elongation at break reaches 2%.
FIG. 5 is a thermal conductivity graph of CNF/BNNS composite films prepared under different BN addition amounts. It can be seen that the thermal conductivity of the composite film is gradually improved with the increase of the addition amount of BN, and when the addition amount of BN is 50wt.%, the thermal conductivity of the composite film can reach 0.188 W.m -1 K -1 ；
Fig. 6 is a temperature reduction curve of a pure CNF film and a CNF/BNNS composite film in which the BN addition amount is 30wt.%, and it can be seen that the heat dissipation performance of the composite film is significantly better than that of the pure CNF film due to the addition of the heat conductive filler.
Example 6:
(1) Weighing macroscopic cellulose fiber slurry containing 1g of oven-dry mass, adding deionized water to 200g, uniformly stirring, and defibering for 5min to obtain suspension containing 0.5wt.% of cellulose fiber for later use.
(2) Magnetically stirring the slurry after the defibering in (1), sequentially adding 0.01g TEMPO (2,2,6,6-tetramethylpiperidine-nitrogen-oxide), 0.01g sodium bromide (NaBr) and 2mmol sodium hypochlorite (NaClO), and adding 0.2 mol/L -1 Adjusting the pH value to 9 with sodium hydroxide (NaOH), oxidizing at room temperature for 4h (keeping the pH value at 9, adjusting the pH value once every 0.5 h), adding 2mL of absolute ethyl alcohol after the reaction is finished, quenching, carrying out vacuum filtration to remove the solvent, washing with deionized water to be neutral, adding water to 200g of the obtained filter cake, and stirring and dispersing to obtain a first dispersion liquid.
(3) Weighing 1g of boron nitride powder, adding the dispersion liquid prepared in the step (2), and uniformly stirring to obtain a second dispersion liquid with the boron nitride addition of 50wt.%.
(4) And (4) ball-milling the dispersion liquid prepared in the step (3) for 9 hours, wherein the ball-material mass ratio is 1:1, and the rotating speed of a ball mill is 400rpm to obtain a third dispersion liquid, and the ball-milling is simple, easy to operate and suitable for large-scale production.
(5) And (3) carrying out ultrasonic treatment on the third dispersion liquid at 500W for 4h, and homogenizing for 30 times under 50MPa to obtain the CNF/BNNS composite dispersion liquid. The ultrasonic treatment is used for preventing the third dispersion liquid from flocculating and influencing the subsequent homogenizing effect; the higher the pressure at homogenization, the smaller the diameter and the larger the aspect ratio of the cellulose cleaved CNF, and the thinner the exfoliated BNNS sheet, but the smaller the lateral dimension.
Example 7:
(1) Weighing macroscopic cellulose fiber slurry containing 1.5g of oven-dry mass, adding deionized water to 100g, uniformly stirring, and defibering for 5min to obtain suspension containing 1.5wt.% of cellulose fiber for later use.
(2) The slurry after the disintegration in (1) was magnetically stirred, 0.03g TEMPO (2,2,6,6-tetramethylpiperidine-nitrogen-oxide), 0.3g sodium bromide (NaBr) and 5mmol sodium hypochlorite (NaClO) were added in this order, and 0.1 mol. L. -1 Adjusting the pH value to 11 with sodium hydroxide (NaOH), oxidizing at room temperature for 4h (keeping the pH value at 11, adjusting the pH value every 0.5 h), adding 5mL of absolute ethyl alcohol after the reaction is finished, quenching, carrying out vacuum filtration to remove the solvent, washing with deionized water to be neutral, adding water to 200g of the obtained filter cake, and stirring and dispersing to obtain a first dispersion.
(3) Weighing 1.5g of boron nitride powder, adding the dispersion liquid prepared in the step (2), and uniformly stirring to obtain a second dispersion liquid with the boron nitride addition of 50wt.%.
(4) And (3) ball-milling the dispersion liquid prepared in the step (3) for 15h, wherein the mass ratio of ball materials is 1.5.
(5) And (3) carrying out ultrasonic treatment on the third dispersion liquid at 700W for 3h, and then homogenizing for 20 times at 100MPa to obtain the CNF/BNNS composite dispersion liquid. The ultrasonic treatment is to prevent the third dispersion liquid from flocculating and influencing the subsequent homogenizing effect; the higher the pressure at homogenization, the smaller the diameter and the larger the aspect ratio of the cellulose cleaved CNF, and the thinner the exfoliated BNNS sheet, but the smaller the lateral dimension.
Claims (7)
1. A preparation method of CNF/BNNS composite dispersion liquid is characterized by comprising the following steps:
s1, TEMPO oxidation is carried out on suspension of macroscopic cellulose fiber slurry, the pH of the suspension is adjusted to be alkaline, absolute ethyl alcohol is added for quenching and suction filtration after oxidation, and water is added into an obtained filter cake for dispersion to obtain first dispersion liquid;
s2, adding boron nitride powder into the first dispersion liquid to obtain a second dispersion liquid, and performing ball milling to obtain a third dispersion liquid;
s3, performing ultrasonic treatment on the third dispersion liquid, and homogenizing to obtain a CNF/BNNS composite dispersion liquid;
in the step S2, 9h to 15h is ball-milled under the conditions that the ball-material mass ratio is (1 to 1.5) to 1 and the rotation speed of the ball mill is 400 to 600 rpm;
in the step S3, the ultrasound is performed for 2 to 4 hours under the conditions of 500 to 700W; the homogenization is to carry out homogenization treatment for 20 to 40 times under the condition of 50 to 100 MPa;
the content of cellulose fibers in the suspension of the macroscopic cellulose fiber slurry is 0.5 wt% -1.5 wt%;
in step S2, the amount of boron nitride added to the second dispersion is 10 wt% to 50 wt%.
2. The method of claim 1, wherein in step S1, the macro cellulose fiber slurry is a slurry made of wood, seed fiber, bast fiber, or grass.
3. The method for preparing the CNF/BNNS composite dispersion liquid according to claim 1, wherein in step S1, 0.01g to 0.03g of TEMPO,0.1g to 0.3g of NaBr and 2mmol to 5mmol of NaClO are sequentially added to the suspension for TEMPO oxidation.
4. According to claim 1The preparation method of the CNF/BNNS composite dispersion liquid is characterized in that in the step S1, 0.1mol multiplied by L is adopted -1 ~0.2 mol×L -1 Adjusting the pH value of the mixed solution to 9-11 with NaOH solution, oxidizing 2 h-4 h, adding 2 mL-5 mL of absolute ethyl alcohol, and quenching, wherein the pH value of the mixed solution is kept at 9-11 during oxidation.
5. A CNF/BNNS composite dispersion, characterized in that it is prepared according to the preparation method of any one of claims 1 to 4.
6. A CNF/BNNS high thermal conductive film, characterized in that, the CNF/BNNS composite dispersion liquid of claim 5 is used for preparing, the thermal conductivity of the CNF/BNNS high thermal conductive film is 0.103W Xm -1 K -1 ~0.188 W×m -1 K -1 The strength is 30MPa to 60MPa, and the elongation at break is 2% to 5%.
7. A preparation method of CNF/BNNS high thermal conductive film, which is characterized in that the method is used for preparing the CNF/BNNS high thermal conductive film of claim 6, and comprises the following steps:
1) Diluting the CNF/BNNS composite dispersion liquid, and performing suction filtration to obtain a filter cake;
2) The obtained filter cake is subjected to cold pressing and drying to obtain a CNF/BNNS high-thermal-conductivity film;
the CNF/BNNS high thermal conductive film is used for packaging electronic equipment.
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| CN107840979A (en) * | 2017-11-14 | 2018-03-27 | 武汉理工大学 | A kind of preparation method of crosslinking nano cellulose/hexagonal boron nitride nanosheet composite membrane |
| CN109971020A (en) * | 2019-03-26 | 2019-07-05 | 上海大学 | A kind of functional nano-fiber element-boron nitride laminated film and preparation method thereof |
| CN113416334A (en) * | 2021-07-09 | 2021-09-21 | 陕西科技大学 | Hydroxyethyl cellulose/boron nitride nano composite film and preparation method thereof |
| CN113737305A (en) * | 2021-10-11 | 2021-12-03 | 陕西科技大学 | Cellulose nanofiber and preparation method and application thereof |
| CN114074927A (en) * | 2020-08-18 | 2022-02-22 | 清华大学深圳国际研究生院 | Two-dimensional material, preparation method thereof and composite membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840979A (en) * | 2017-11-14 | 2018-03-27 | 武汉理工大学 | A kind of preparation method of crosslinking nano cellulose/hexagonal boron nitride nanosheet composite membrane |
| CN109971020A (en) * | 2019-03-26 | 2019-07-05 | 上海大学 | A kind of functional nano-fiber element-boron nitride laminated film and preparation method thereof |
| CN114074927A (en) * | 2020-08-18 | 2022-02-22 | 清华大学深圳国际研究生院 | Two-dimensional material, preparation method thereof and composite membrane |
| CN113416334A (en) * | 2021-07-09 | 2021-09-21 | 陕西科技大学 | Hydroxyethyl cellulose/boron nitride nano composite film and preparation method thereof |
| CN113737305A (en) * | 2021-10-11 | 2021-12-03 | 陕西科技大学 | Cellulose nanofiber and preparation method and application thereof |
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