阅读说明：本技术 一种导热纺织材料的制备方法 (Preparation method of heat-conducting textile material ) 是由 程晓敏 李林峰 李元元 于 2020-12-10 设计创作，主要内容包括：本发明涉及一种高导热纺织品的制备方法,包括如下步骤：(1)将纺织品置于多巴胺溶液中浸泡处理后,取出烘干；(2)在步骤(1)所得纺织品的表面采用原子层沉积设备生成均匀、致密的导热材料涂层,从而得到导热纺织材料。该方法对各种纺织材料的加工处理均适用,具有均匀、厚度可控、精度高的特点,也不会影响纺织品原有的手感、柔顺及光泽；且原料用量极少,沉积过程中不会产生水溶液,生产时对环境污染小,工艺流程少,操作过程方便易控。(The invention relates to a preparation method of a high-thermal-conductivity textile, which comprises the following steps: (1) soaking the textile in a dopamine solution, taking out and drying; (2) and (2) generating a uniform and compact heat conduction material coating on the surface of the textile obtained in the step (1) by adopting atomic layer deposition equipment, thereby obtaining the heat conduction textile material. The method is suitable for processing various textile materials, has the characteristics of uniformity, controllable thickness and high precision, and does not influence the original hand feeling, smoothness and luster of the textile; and the raw material consumption is very little, no aqueous solution is generated in the deposition process, the environmental pollution is little during the production, the process flow is few, and the operation process is convenient and easy to control.)

1. A preparation method of a heat-conducting textile material is characterized by comprising the following steps:

(1) soaking the textile in a dopamine solution, taking out and drying;

(2) and (2) generating a uniform and compact heat conduction material coating on the surface of the textile obtained in the step (1) by adopting atomic layer deposition equipment, thereby obtaining the heat conduction textile material.

2. The method for preparing the heat-conducting textile material according to claim 1, wherein in the step (1), the dopamine solution is 2-10% dopamine aqueous solution.

3. The preparation method of the heat-conducting textile material according to claim 1, wherein in the step (1), the bath ratio of the textile to the dopamine solution is 1: 1-10.

4. The method for preparing a heat-conducting textile material according to claim 1, wherein in the step (1), the soaking treatment is performed simultaneously with the ultrasonic treatment or the vibration treatment or the stirring treatment so as to maintain the uniformity of the dopamine solution during the soaking process.

5. The method according to claim 1, wherein in the step (2), the heat conductive material coating is a coating formed by one or more of aluminum oxide, aluminum nitride, zinc oxide, boron nitride, silicon carbide, nickel oxide and other heat conductive materials.

6. The method according to claim 1, wherein in the step (2), during the atomic layer deposition, according to the difference of the required thermal conductive material coating, the corresponding precursor is selected and introduced into the atomic deposition device to deposit the corresponding thermal conductive material on the textile surface and form the coating.

7. The method according to claim 6, wherein in the step (2), the deposition of the atomic layer comprises two precursors, and the precursors of the thermal conductive materials, namely alumina, aluminum nitride, zinc oxide, boron nitride, silicon carbide and nickel oxide, correspond to trimethylaluminum and water, aluminum trichloride and ammonia, diethylzinc and water, trimethylboron and ammonia, silicon tetrachloride and acetylene, nickelocene and ozone, respectively.

8. The method for preparing a heat-conducting textile material according to claim 1, wherein in the step (2), the parameters of the atomic layer deposition are as follows: the reaction temperature is 70-150 ℃, the single-cycle reaction time is 10-70 s, the purging gas is protective atmosphere such as high-purity nitrogen or helium or argon, and the total reaction time is up to the coating thickness of 1-100 nm.

9. The method for preparing the heat-conducting textile material according to claim 6, wherein the textile is one or more of fibers, yarns, fabrics and non-woven fabrics, and the raw material of the textile is one or more of cotton, wool, hemp, silk, rayon and synthetic fibers.

Technical Field

The invention relates to a preparation method of a heat-conducting textile material, and belongs to the technical field of textile material processing.

Background

Cool textiles have been the focus of attention of researchers as textile materials that can provide a cool feeling in summer, and the cool characteristics can be realized by imparting high thermal conductivity to the textile materials. In addition, the heat conduction material plays a role in electronic products, can transmit heat generated by the electronic device during working to the outside, plays a role in heat dissipation, greatly improves the working efficiency of the electronic device, and can eliminate a series of potential safety hazards caused by temperature rise. The rapid progress of electronic technology has led to the increasingly strict requirements for heat-conducting materials, which are required to be flexible, light, bendable and insulating in some very precise electronic instruments, and textile materials have various characteristics, so that the textile materials become the most qualified base materials. If the textile material is subjected to heat conduction treatment, the method can be applied to various fields, and the application value of the textile material can be greatly improved.

Currently, there are few studies on heat-conductive textile materials, and all have limitations. In the article "graphene ultraviolet-proof, electric-conduction and heat-conduction functional finishing of pure cotton fabric" in the 9 th phase of "printing and dyeing", a treatment method for covering graphene on cotton textiles is described, and the heat-conduction performance of the modified cotton fabrics is greatly improved. However, the cost of graphene is high, and a graphene aqueous solution needs to be prepared; in addition, since graphene is coated on the surface of the fabric by padding, the durability is not high.

In addition, in an article "High temperature thermal composite textile by" green "electrospinning" of the 10 th year 2018 of Nanoscale, a heat-conducting nanocomposite textile material is constructed by boron nitride (FBN) nanosheets and Polyimide (PI) nanofibers through experimental research, and the method has the disadvantages of complicated steps, harsh conditions and inconvenience for large-scale industrial production; and the method can only prepare heat-conducting filaments, and cannot realize heat-conducting treatment on textiles such as yarns, fabrics and the like.

Disclosure of Invention

The technical problem to be solved by the invention is to provide a preparation method of a heat-conducting textile material aiming at the defects in the prior art, which has broad spectrum, is easy to prepare various textiles, has high heat conductivity coefficient, and is convenient and easy to control in the operation process.

The technical scheme adopted by the invention for solving the problems is as follows:

a preparation method of a heat-conducting textile material comprises the following steps:

(1) soaking the textile in a dopamine solution, taking out and drying;

(2) and (2) generating a uniform and compact heat conduction material coating on the surface of the textile obtained in the step (1) by adopting atomic layer deposition equipment, thereby obtaining the heat conduction textile material.

According to the scheme, in the step (1), the dopamine solution is a dopamine aqueous solution with the concentration of 2-10%.

According to the scheme, in the step (1), the bath ratio of the textile to the dopamine solution is 1: 1-10, namely the mass ratio of the textile to the dopamine solution is 1: 1-10.

According to the scheme, in the step (1), ultrasonic treatment, oscillation treatment, stirring treatment and the like are adopted during soaking treatment so as to keep the uniformity of the dopamine solution in the soaking process.

According to the scheme, in the step (2), the heat conducting material coating is a coating formed by one or more of aluminum oxide, aluminum nitride, zinc oxide, boron nitride, silicon carbide, nickel oxide and other heat conducting materials. During atomic layer deposition, according to the difference of the required heat conduction material coating, selecting corresponding precursors to be introduced into atomic deposition equipment, controlling reaction temperature, reaction time and the like, depositing corresponding heat conduction materials on the surface of the textile and forming the coating.

According to the scheme, in the step (2), the parameters of the atomic layer deposition are as follows: the reaction temperature is 70-150 ℃, the single-cycle reaction time is 10-70 s, the purging gas is protective atmosphere such as high-purity nitrogen or helium or argon, and the total reaction time is up to the coating thickness of 1-100 nm.

Preferably, the heat conducting material coating is a coating formed by one or more of aluminum oxide, aluminum nitride, zinc oxide, boron nitride, silicon carbide, nickel oxide and other heat conducting materials.

Preferably, the precursors for atomic layer deposition are generally two, for example, the precursors for thermal conduction materials of aluminum oxide, aluminum nitride, zinc oxide, boron nitride, silicon carbide, and nickel oxide correspond to trimethylaluminum and water, aluminum trichloride and ammonia, diethylzinc and water, trimethylboron and ammonia, silicon tetrachloride and acetylene, nickelocene, and ozone, respectively.

In the invention, the textile is one or more of fiber, yarn, fabric, non-woven fabric and the like, and the raw material of the textile can be one or more of cotton, wool, hemp, silk (silk and the like), artificial fiber, synthetic fiber and the like. The artificial fiber comprises viscose fiber, acetate fiber, cuprammonium fiber, etc., and the synthetic fiber comprises terylene, chinlon, polypropylene fiber or nylon, acrylic fiber, etc. The method is particularly suitable for textile materials rich in active groups such as hydroxyl groups, amino groups and the like, such as cellulose fibers such as cotton, hemp, viscose and the like, wool, silk and yarns and fabrics made of the wool, the silk and the like.

Compared with the prior art, the invention has the beneficial effects that:

1. after the dopamine solution is pretreated, the textile is directly placed in atomic layer deposition equipment for coating deposition, and the heat-conducting textile material can be obtained. The method is suitable for processing various textile materials, has the characteristics of uniformity, controllable thickness and high precision, and does not influence the original hand feeling, smoothness and luster of the textile; and the raw material consumption is very little, no aqueous solution is generated in the deposition process, the environmental pollution is little during the production, the process flow is few, and the operation process is convenient and easy to control.

2. The invention needs to adopt dopamine to pretreat the textile body in advance, increases the surface activity of the textile body, and is beneficial to enhancing the firmness and the bonding force of the textile material and the heat conduction material coating deposited by the atomic layer.

3. The invention adopts the atomic layer deposition technology to carry out heat conduction material coating on the textile body, and particularly, two precursors required by the heat conduction coating material are alternately introduced into a reaction chamber, chemical adsorption reaction is carried out on the textile body to form the heat conduction coating material, and the control of the thickness of the coating material is realized by adjusting the cycle number of the reaction. Atomic layer deposition is a widely used technology in the field of electronic semiconductors, but rarely is it related to the field of textile processing. The invention adopts the accurately-regulated atomic layer deposition technology, creatively combines dopamine which is a material capable of effectively improving the binding force between material interfaces, and enables the coating material to be uniformly and firmly combined on the surface of the textile body, so that the body can have higher heat-conducting property even if a trace amount of the coating material is used, and the body has higher wear-resisting property. In addition, the mechanical property of the textile body is strengthened due to the adhesion of the coating material; the corrosion resistance of the textile can be effectively improved.

Drawings

Fig. 1 is a scanning electron microscope image of the heat-conductive textile material, heat-conductive cotton fabric, prepared in example 1 and comparative example 1; wherein, (1) example 1; (2) comparative example 1.

Detailed Description

In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.

Example 1

A preparation method of a heat-conducting textile material specifically comprises the following steps:

A. cotton fabric pretreatment: dissolving dopamine in deionized water to prepare a 2% dopamine solution, then placing a clean cotton fabric in the dopamine solution, controlling the bath ratio of the cotton fabric to the dopamine solution to be 1:10, ultrasonically oscillating the cotton fabric for 24 hours at normal temperature, and taking out and drying the cotton fabric;

B. and (3) cotton fabric heat conduction treatment: b, generating a uniform and compact aluminum oxide heat conduction material coating on the surface of the cotton fabric obtained in the step A by utilizing atomic layer deposition equipment; the deposition process is as follows:

opening an atomic layer deposition device, and alternately introducing pulses of a gas-phase trimethylaluminum precursor and a water precursor, wherein the exposure time of trimethylaluminum and the exposure time of water are respectively 0.2s and 0.8s, the reaction time is 9.5s, the purging gas is high-purity nitrogen, the purging time is 25s, the reaction temperature is 70 ℃, and after 6 ALD (single cycle reaction time is 70s), an alumina coating with the thickness of 1nm, which is compact and uniform (the growth rate of alumina is 0.16 nm/cycle) is formed on the surface of the cotton fabric, so that the heat-conducting textile material, namely the heat-conducting cotton fabric, is obtained.

Test results show that the heat conductivity coefficient of the heat-conducting cotton fabric prepared in example 1 can reach 0.11W/m K, and is increased by more than 20% compared with that of the original cotton fabric.

Comparative example 1

The difference from example 1 is that: step a is omitted.

Compared with the example 1, the heat-conducting cotton fabric prepared under the same atomic layer deposition conditions in the comparative example 1 without the dopamine solution treatment has the heat conductivity coefficient of 0.102W/m K.

As shown in fig. 1, the surface coating of the thermal conductive cotton fabric prepared in example 1 is more uniform, flat and firm than that of comparative example 1. The method for preparing the heat-conducting textile material, disclosed by the invention, has the advantages that the textile body is pretreated by dopamine in advance, so that the firmness and the bonding force of the textile material and the heat-conducting material coating deposited by the atomic layer can be enhanced, and the surface of the fabric is more uniform and flat.

Example 2

A preparation method of a heat-conducting textile material specifically comprises the following steps:

A. polyester yarn pretreatment: dissolving dopamine in deionized water to prepare a 10% dopamine solution, then placing clean polyester yarns in the dopamine solution, controlling the bath ratio of the polyester yarns to the dopamine solution to be 1:1, ultrasonically oscillating for 12h at normal temperature, taking out and drying;

B. conducting heat treatment on polyester yarns: b, generating a uniform and compact zinc oxide heat conduction material coating on the surface of the polyester yarn obtained in the step A by utilizing atomic layer deposition equipment; the deposition process is as follows:

opening an atomic layer deposition device, and alternately introducing pulses of a gas-phase diethyl zinc precursor and a water precursor, wherein the exposure time of diethyl zinc and the exposure time of water are respectively 0.05s and 0.15s, the reaction time is respectively 0.9s, the purging gas is high-purity helium, the purging time is respectively 4s, the reaction temperature is 150 ℃, and after 1500 ALD (single cycle reaction time is 10s), a compact and uniform zinc oxide coating with the thickness of 100nm is formed on the surface of the polyester yarn (the growth rate of zinc oxide is 0.066 nm/cycle), so that the heat-conducting textile material, namely the heat-conducting polyester yarn, is obtained.

The test result shows that the heat diffusion coefficient of the heat-conducting polyester yarn prepared in the example 2 reaches 1.42 x 10^-7m²And/s is increased by more than 20 percent compared with the initial polyester yarn.

Comparative example 2

The difference from example 2 is that: step a is omitted.

Compared with example 2, comparative example 2 does not adopt dopamine solution treatment, and the thermal conductive polyester yarn prepared under the same atomic layer deposition condition has the thermal diffusivity of 1.33 x 10^-7m²/s。

Example 3

A preparation method of a heat-conducting textile material specifically comprises the following steps:

A. polyester filament yarn pretreatment: dissolving dopamine in deionized water to prepare 6% dopamine solution, then placing clean polyester filaments in the dopamine solution, controlling the bath ratio of the polyester filaments to the dopamine solution to be 1:5, ultrasonically oscillating for 18h at normal temperature, taking out and drying;

B. conducting heat treatment on polyester filaments: b, generating a uniform and compact aluminum nitride heat conduction material coating on the surface of the polyester filament yarn obtained in the step A by utilizing atomic layer deposition equipment; the deposition process is as follows:

opening an atomic layer deposition device, alternately introducing pulses of a gas-phase aluminum trichloride precursor and an ammonia precursor, wherein the exposure time of the aluminum trichloride and the ammonia is 0.1s and 0.5s respectively, the reaction time is 3.4s and 6s respectively, the reaction temperature is 110 ℃, the purging gas is high-purity nitrogen, the purging time is 15s, forming a compact and uniform aluminum nitride coating (the growth rate of the aluminum nitride is 0.083 nm/cycle) with the thickness of 50nm on the surface of the polyester filament yarn through 600 ALD cycles (the single cycle reaction time is 40s) to obtain the heat-conducting textile material, namely the heat-conducting polyester filament yarn, then soaking the heat-conducting polyester filament yarn in a KH580 silane coupling agent with the concentration of 10% for hydrolysis resistance, and then drying.

The test result shows that the axial heat conductivity coefficient of the heat-conducting polyester filament yarn obtained in the example 3 can reach 1.27W/m × K, and is increased by more than 35% compared with the initial polyester filament yarn.

Comparative example 3

The difference from example 3 is that: step a is omitted.

Compared with example 3, comparative example 3 does not adopt dopamine solution treatment, and the axial thermal conductivity coefficient of the thermal conductive textile material-thermal conductive polyester filament prepared under the same atomic layer deposition condition is 1.25W/m × K.

Example 4

A preparation method of a heat-conducting textile material specifically comprises the following steps:

A. pretreatment of nylon non-woven fabric: dissolving dopamine in deionized water to prepare a 4% dopamine solution, then placing a clean nylon non-woven fabric in the dopamine solution, controlling the bath ratio of the nylon non-woven fabric to the dopamine solution to be 1:8, ultrasonically oscillating at normal temperature for 20 hours, taking out and drying;

B. heat conduction treatment of nylon non-woven fabric: b, generating a uniform and compact boron nitride heat conduction material coating on the surface of the nylon non-woven fabric obtained in the step A by utilizing atomic layer deposition equipment; the deposition process is as follows:

opening an atomic layer deposition device, and alternately introducing pulses of a gas-phase trimethylboron precursor and an ammonia precursor, wherein the exposure time of trimethylboron and ammonia is 0.25s, the reaction time is 4.75s, the reaction temperature is 130 ℃, the purging gas is high-purity helium, the purging time is 10s, and after 1000 ALD cycles (the reaction time of a single cycle is 30s), a compact and uniform boron nitride coating with the thickness of 70nm (the growth rate of boron nitride is 0.07 nm/cycle) is formed on the surface of the nylon non-woven fabric, so that the heat-conducting textile material-nylon heat-conducting non-woven fabric is obtained.

The test result shows that the heat conductivity coefficient of the heat-conducting nylon non-woven fabric obtained in the example 4 can reach 0.33W/m K, and is increased by more than 35% compared with that of the original nylon non-woven fabric.

Comparative example 4

The difference from example 4 is that: step a is omitted.

Compared with example 4, comparative example 4 does not adopt dopamine solution treatment, and the heat conduction nylon non-woven fabric prepared under the same atomic layer deposition condition has the heat conduction coefficient of 0.31W/m K.

Example 5

A preparation method of a heat-conducting textile material specifically comprises the following steps:

A. pretreating polypropylene fabrics: dissolving dopamine in deionized water to prepare 8% dopamine solution, then placing clean polypropylene fabric in the dopamine solution, controlling the bath ratio of the polypropylene fabric to the dopamine solution to be 1:4, ultrasonically oscillating at normal temperature for 16h, taking out and drying;

B. and (3) polypropylene fabric heat conduction treatment: b, generating a uniform and compact silicon carbide heat conduction material coating on the surface of the polypropylene fabric obtained in the step A by utilizing atomic layer deposition equipment; the deposition process is as follows:

opening an atomic layer deposition device, and alternately introducing pulses of a gas-phase silicon tetrachloride precursor and an acetylene precursor, wherein the exposure time of silicon tetrachloride and acetylene is 0.15s, the reaction temperature is 80 ℃, the reaction time is 6s, the purging gas is high-purity nitrogen, the purging time is 24s, and after 250 ALD cycles (the single cycle reaction time is 60.3s), a compact and uniform silicon carbide coating with the thickness of 20nm is formed on the surface of the polypropylene fabric (the growth rate of silicon carbide is 0.08 nm/cycle), so that the heat-conducting textile material, namely the heat-conducting polypropylene fabric, is obtained.

The test results show that the thermal conductivity of the thermal conductive polypropylene fabric prepared in example 5 can reach 0.32W/m × K, which is increased by more than 29% compared with the original polypropylene fabric.

Comparative example 5

The difference from example 5 is that: step a is omitted.

Compared with example 5, comparative example 5 has no dopamine solution treatment, and the thermal conductivity coefficient of the thermal conductive polypropylene fabric prepared under the same atomic layer deposition condition is 0.30W/m K.

Example 6

A preparation method of a heat-conducting textile material specifically comprises the following steps:

A. pretreating viscose fibers: dissolving dopamine in deionized water to prepare 5% dopamine solution, then placing clean viscose fiber in the dopamine solution, controlling the bath ratio of the viscose fiber to the dopamine solution to be 1:6, ultrasonically oscillating at normal temperature for 19h, taking out and drying;

B. conducting heat treatment on viscose fibers: b, generating a uniform and compact nickel oxide heat conduction material coating on the surface of the viscose fiber obtained in the step A by utilizing atomic layer deposition equipment; the deposition process is as follows:

opening an atomic layer deposition device, and alternately introducing gas-phase nickel-metallocene precursor and ozone precursor pulses, wherein the exposure time of the nickel-metallocene and the ozone is 0.05s, the reaction time is 4s, the reaction temperature is 90 ℃, the purging gas is high-purity nitrogen, the purging time is 20s, and after 500 ALD cycles (the reaction time of a single cycle is 48.1s), a compact and uniform nickel oxide coating with the thickness of 60nm is formed on the surface of the viscose fiber (the growth rate of the nickel oxide is 0.12 nm/cycle), so that the heat-conducting textile material, namely the heat-conducting viscose fiber, is obtained.

The test result shows that the thermal conductivity coefficient of the thermal conductive viscose fiber obtained in example 6 can reach 0.075W/m K, and is increased by more than 24% compared with the initial viscose fiber.

Comparative example 6

The difference from example 6 is that: step a is omitted.

Compared with example 6, comparative example 6 has no dopamine solution treatment, and the thermal conductivity coefficient of the thermal conductive viscose fiber prepared under the same atomic layer deposition condition is 0.067W/m.multidot.K.

The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.