阅读说明：本技术 一种陶瓷表面黑色分子吸附层微波烧结制备方法 (Microwave sintering preparation method of black molecular adsorption layer on ceramic surface ) 是由 魏强 潘娅婷 院小雪 张立宪 于 2019-10-17 设计创作，主要内容包括：本发明公开了一种陶瓷表面黑色分子吸附层微波烧结制备方法,该方法包括对陶瓷基体表面亲水化处理；将分子筛、黑化剂和黑色二氧化钛按比例混合球磨后,均匀溶于去离子水得到涂覆液；将陶瓷浸渍于涂覆液中,形成分子筛/黑化剂涂层；最后将涂覆黑化吸附层的陶瓷置于微波炉中烧结制备。相对于传统的陶瓷表面分子筛膜制备工艺,本发明采用微波烧结工艺在陶瓷基体表面制备分子筛/黑化剂吸附涂层,改良了烧结工艺,制备时间短,成本较低,对环境污染小,吸附特殊密闭环境内的有害气体；该涂层为黑色,可降低光的散射作用；涂层具有一定的吸附能力；涂层结合力不易剥落,无粉末飞扬,具有绿色环保等优点。(The invention discloses a microwave sintering preparation method of a black molecular adsorption layer on a ceramic surface, which comprises the following steps of carrying out hydrophilization treatment on the surface of a ceramic matrix; mixing and ball-milling a molecular sieve, a blackening agent and black titanium dioxide according to a proportion, and uniformly dissolving in deionized water to obtain a coating solution; dipping the ceramic into the coating liquid to form a molecular sieve/blackening agent coating; and finally, placing the ceramics coated with the blackening adsorption layer in a microwave oven for sintering preparation. Compared with the traditional preparation process of the molecular sieve membrane on the ceramic surface, the invention adopts the microwave sintering process to prepare the molecular sieve/blackening agent adsorption coating on the surface of the ceramic substrate, improves the sintering process, has short preparation time, lower cost and little pollution to the environment, and adsorbs harmful gases in a special closed environment; the coating is black, so that the scattering effect of light can be reduced; the coating has certain adsorption capacity; the coating has the advantages of difficult peeling of binding force, no flying of powder, environmental protection and the like.)

1. A microwave sintering preparation method of a black molecular adsorption layer on a ceramic surface comprises the following steps:

the method comprises the following steps: carrying out hydrophilization treatment on the ceramic surface;

step two: mixing and ball-milling a molecular sieve, a blackening agent and black titanium dioxide according to a mass ratio of 1:5:1-1:8:1.5, and uniformly dissolving in deionized water to obtain a coating solution;

step three: dipping the ceramic into the coating liquid to form a molecular sieve/blackening agent coating;

step four: sintering and forming in a microwave oven.

2. The microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface according to claim 1, wherein in the first step, the hydrophilization treatment of the ceramic surface is performed by soaking the ceramic surface in a nitric acid solution with a temperature of 30-65 ℃ and a concentration of 10-50%.

3. The microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface according to claim 1, wherein in the first step, the hydrophilization treatment of the ceramic surface is performed by using a jet low-temperature plasma treatment with oxygen with a concentration of 20-100% as a gas source.

4. The microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface according to claim 1, wherein in the second step, the molecular sieve is a mixture of any one or more of X type, A type and ZSM type.

5. The microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface according to claim 1, wherein in the second step, the blackening agent is any one or more of carbon black, silicon carbide and carbon nanotubes.

6. The microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface according to claim 1, wherein in the fourth step, the frequency of microwave heating is 0.9GHz-5.8GHz, and the time of microwave sintering is 72s-480 s.

7. The microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface according to claim 1, wherein the thickness of the black molecular adsorption coating is less than 3 μm.

Technical Field

The invention relates to the field of inorganic material microwave sintering, in particular to a method for preparing a molecular sieve and blackening agent composite molecular adsorption coating on a ceramic matrix by using a microwave sintering technology.

Background

In recent years, with the rapid development of economy and society of China, the problem of gas pollution is increasingly serious. Particularly, in a closed space environment where material exchange with the outside cannot be performed, such as an automobile, a submarine, a space station and the like, a trace amount of harmful gas is inevitably generated due to material outgassing, equipment operation and the like, and a serious damage effect can be generated after continuous accumulation. Therefore, the problem of harmful gas in the enclosed space is receiving much attention.

For harmful gases in a closed environment, adsorbents such as activated carbon, activated carbon fibers and molecular sieves with high specific surface area, large adsorption capacity, stable performance and low cost can be selected for adsorption. Compared with the active carbon with poor mechanical property and the active carbon fiber which can only adsorb nonpolar molecules, the molecular sieve formed by the framework of the silicon-oxygen tetrahedron and the aluminum-oxygen tetrahedron has very large dispersion force and electrostatic force on the surface, and can effectively adsorb all organic molecules with the diameter smaller than the aperture of the molecular sieve through regular pore passages and cavities. Therefore, the adsorption coating prepared by taking the molecular sieve as the raw material has a wide application prospect.

The molecular sieve adsorption coating has excellent performance and can adsorb a large amount of harmful gases, but the molecular sieve coating is white, and the damage of light scattering to instrument lenses and the like cannot be avoided in special closed environments sensitive to light such as the instrument lenses and the like. Therefore, it is important to explore the method for preparing black adsorption coating.

Disclosure of Invention

Carbon black, silicon carbide, carbon nanotubes and the like are excellent wave-absorbing materials, can generate a large amount of heat in a short time under a microwave environment to reach a sintering temperature, can form a black adsorption coating after being mixed and sintered with a molecular sieve in a certain proportion, and absorbs stray light to protect devices in a closed environment. According to the microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface, provided by the invention, the molecular sieve/blackening agent adsorption coating is prepared on the surface of the ceramic substrate by adopting a microwave sintering process, so that the time cost is effectively saved, and harmful gases in a special closed environment are adsorbed.

The invention aims to provide a black molecule adsorption layer on the surface of ceramic, which adsorbs harmful gas molecules in a closed environment and absorbs and reduces the influence of stray light. Introduction of black TiO₂The blackening effect is increased, and the composite powder is effectively dispersed in the deionized water on the premise of not introducing organic matters. The microwave sintering preparation method is adopted to realize the sintering preparation of the adsorption coating rapidly and with low cost. The blackening agent has the characteristic of microwave absorption, and under the action of microwaves, according to the dipole rotation polarization principle, molecules of the blackening agent generate friction-like motion along with the change of positive and negative poles in an electric field, a large amount of heat is rapidly generated among the molecules, and the heat is transferred to the molecular sieve, so that the composite material is heated from inside to outside, and a uniform black molecular adsorption coating is formed.

In order to achieve the purpose, the microwave sintering preparation method of the black molecular adsorption layer on the surface of the ceramic provided by the invention comprises the following steps:

the method comprises the following steps: carrying out hydrophilization treatment on the ceramic surface;

step two: mixing and ball-milling a molecular sieve, a blackening agent and black titanium dioxide according to a mass ratio of 1:5:1-1:8:1.5, and uniformly dissolving in deionized water to obtain a coating solution;

step three: dipping the ceramic into the coating liquid to form a molecular sieve/blackening agent coating;

step four: sintering and forming in a microwave oven.

Further, the microwave sintering preparation method of the black molecular adsorption layer on the ceramic surface comprises the following steps of firstly, soaking the ceramic surface in a 10-50% nitric acid solution at the temperature of 30-65 ℃ for hydrophilization treatment; or jet low-temperature plasma treatment with 20-100% oxygen as gas source.

In the second step, the molecular sieve is a mixture of any one or more of X type, A type and ZSM type. The blackening agent is any one or more of carbon black, silicon carbide and carbon nano tubes.

In the fourth step, the frequency of microwave heating is 0.9GHz-5.8GHz, and the time of microwave sintering is 72s-480 s.

Compared with the existing ceramic surface molecular adsorption coating, the molecular sieve/blackening agent composite black molecular adsorption coating has the following advantages:

(1) the preparation of the black molecular adsorption coating has low requirement on equipment, the price of raw materials is low, and the operation process is simple and easy to implement;

(2) the black molecule adsorption coating reduces the sintering time, the internal structure of the coating is more uniform through microwave sintering, and the binding force between the coating and the ceramic surface is increased;

(3) the black molecular adsorption coating ensures the adsorption performance of the molecular sieve, reduces the scattering effect of light, and effectively increases the possibility of the application of the black molecular adsorption coating in the fields of optics, aerospace and the like.

Drawings

FIG. 1 is a macroscopic view of a ceramic-based black molecular adsorption coating;

FIG. 2 is an X-ray diffraction analysis chart of the black molecular adsorption coating in example 1;

FIG. 3 is the adsorption test isothermal adsorption-desorption curve of the black molecular adsorption coating in example 1, where 1 is N₂An adsorption curve; 2 is N₂Desorption profile.

Detailed Description

The invention will be further described with reference to the following figures and specific examples, which are not intended to limit the invention in any way.

The invention relates to a microwave sintering preparation method of a black molecular adsorption layer on a ceramic surface, which mainly comprises the following steps:

hydrophilization treatment of ceramic surface: soaking with 10-50% nitric acid solution at 30-65 deg.C, or using jet low temperature plasma with oxygen concentration of 20-100% as gas source;

preparing a coating solution: weighing molecular sieve, black TiO and black TiO₂The mass ratio of the components is 1:5:1-1:8:1.5, ball-milling, dissolving in deionized water, and uniformly stirring, wherein the blackening agent is black silicon carbide, and the proportion of the components of the coating liquid can be controlled to finally form a black molecular adsorption coating with the thickness of less than 3 mu m on the surface of the ceramic.

Dipping the ceramic into the coating liquid to form a molecular sieve/blackening agent coating;

sintering and forming in a microwave oven, wherein the microwave heating frequency is 0.9GHz-5.8GHz, the microwave heating time is 72s-480s, and finally forming a black molecular adsorption coating with the thickness of less than 3 mu m on the ceramic surface.