Colored basalt fiber resistant to extreme high temperatures and method of making same

Abstract

The application provides a color basalt fiber resistant to extreme high temperature and a preparation method thereof, and the basalt fiber comprises a structural film coated on the surface of the basalt fiber, and the structural film comprises one of a metal element film, a metal oxide film, a composite film of different metal elements or metal oxides, and a composite film of a metal element and a metal oxide; the structural film and the basalt fiber and different film layers of the structural film are combined in a chemical bonding mode. Through the preparation method, the structural film with strong interfacial bonding force, closely combined film layers, resistance to extreme high temperature and different colors is obtained on the surface of the basalt fiber; the metal element film and / or the metal oxide film are loaded on the surface of the basalt fiber, so that the flame-retardant nanocrystal with stable structure is formed on the surface of the fiber, the basalt fiber is endowed with the resistance to extreme high temperature, the problem that the basalt fiber cannot be colored is solved, and the application field of the basalt fiber is widened.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of basalt fiber, and particularly relates to a color basalt fiber resistant to extreme high temperature and a preparation method thereof. BACKGROUND

[0002] With the continuous progress of science and technology, the fiber industry has developed rapidly, and textile materials have become increasingly colorful, with increasing varieties, continuously improved performance and expanding application range. As a new type of fiber, basalt fiber is widely used in military and civilian fields such as aerospace, construction, chemical industry, medicine, electronics and agriculture due to its excellent properties such as high strength, high modulus, corrosion resistance, oxidation resistance, radiation resistance, heat and sound insulation, fire resistance, good filtration and high and low temperature resistance. At the same time, basalt fiber also has the softness and processability of traditional textile fibers, so basalt fiber can also be applied to the field of textile and clothing.

[0003] A basalt fiber and a preparation method thereof are disclosed in Chinese patent (CN 114477756A), which has a relatively high tensile strength by raw material screening. A reinforced basalt fiber impregnant and a preparation method thereof are disclosed in Chinese patent (CN 113480199A), which improves the mechanical strength of basalt fiber by using double-layer microcapsule particles to repair cracks on the surface of basalt fiber. A magnetic basalt fiber and a preparation method thereof are disclosed in Chinese patent (CN 113089133A), which obtains a magnetic basalt fiber with high magnetism and high strength by using 1.5-2.0 wt% Fe 3+ and more than 65 wt% SiO2+Al2O3 through a series of steps. 2+

[0004] It can be seen that a series of methods for preparing basalt fiber with excellent strength performance have been developed in the prior art, and the effect is relatively significant. However, basalt fiber has a single color when used as a textile fiber, and although basalt fiber has high temperature resistance, it still burns in an extreme high temperature environment, which is not conducive to the application of basalt fiber in an extreme high temperature environment, such as fire fighting clothes, fireproof clothes, fire extinguishing blankets and the like.

[0005] Therefore, it is necessary to design an improved color basalt fiber resistant to extreme high temperature and a preparation method thereof to solve the above problems. SUMMARY

[0006] ​The application aims to provide a color basalt fiber resistant to extreme high temperature and a preparation method thereof.

[0007] To achieve the above-mentioned application purposes, the application provides a color basalt fiber resistant to extreme high temperature, which comprises a basalt fiber and a structural film coated on the surface of the basalt fiber, wherein the structural film comprises one of a metal element film, a metal oxide film, a composite film of different metal elements or metal oxides, and a composite film of a metal element and a metal oxide; the structural film and the basalt fiber, and different film layers of the structural film are combined in a chemical bonding manner.

[0008] As a further improvement of the application, when the structural film is a metal element film or a metal oxide film, the difference in refractive index between the metal element film or the metal oxide film and the basalt fiber is at least 0.17; when the structural film is a composite film, the difference in refractive index between different film layers in the composite film is at least 0.17; and the refractive index of the metal element film or the metal oxide film is greater than 1.76.

[0009] As a further improvement of the application, the structural film is a composite film of a metal element and a metal oxide, the metal elements in the metal element and the metal oxide are the same or different; the total thickness of the structural film is 10-300 nm; and the thickness ratio of the film layer formed by the metal element to the film layer formed by the metal oxide in the composite film is (1-6):(1-6).

[0010] As a further improvement of the application, the material of the structural film is one or more of group IIIA elements, group IVA elements except carbon, group IB elements, group IIB elements, group IIIB elements, group IVB elements, group VB elements, group VIB elements, group VIII elements, or one or more of metal oxides thereof.

[0011] As a further improvement of the application, the group IIA element is Mg, the group IIIA element is Al or Ga, the group IVA element is Si, the group IB element is Ag, the group IIB element is Zn, the group IIIB element is Y or Ce, the group IVB element is Ti, Zr or Hf, the group VB element is V or Ta, the group VIB element is Mo or W, and the group VIII element is Co or Pt.

[0012] A preparation method of the color basalt fiber resistant to extreme high temperature according to any one of the above-mentioned application, which comprises the following steps:

[0013] S1, placing the cleaned basalt fiber in a micro-etching solution, reacting for 10-60 min, and then placing it in a plasma cleaning machine for surface treatment for 2-10 min;

[0014] S2, loading a metal element film and / or a metal oxide film on the surface of the basalt fiber treated in step S1 to obtain a colored basalt fiber resistant to extreme high temperature; the metal element film or the metal oxide film and the basalt fiber are combined in a chemically bonded manner, and a structural film is formed on the surface of the basalt fiber, with a thickness of 10-300 nm.

[0015] As a further improvement of the present application, in step S1, the micro-etching solution comprises one of a NaOH solution, dilute hydrochloric acid, or a mixed solution of dilute hydrochloric acid and dilute sulfuric acid; the reaction time of micro-etching is 10-60 min, and the micro-etching solution is preferably a NaOH solution.

[0016] As a further improvement of the present application, in step S2, the method for loading the structural film on the surface of the basalt fiber is specifically:

[0017] The method for loading the metal element film is to use a metal element as a target material, and under the action of an electric field, the metal element is bombarded to the surface of the basalt fiber to deposit and form a basalt fiber loaded with a metal element film;

[0018] The method for loading the metal oxide film is to use argon as a working gas and oxygen as a reaction gas in a reaction chamber, and under the action of an electric field, metal atoms and oxygen atoms react to form an oxide, thereby forming a basalt fiber loaded with a metal oxide film;

[0019] The method for loading the metal element film is combined with the method for loading the metal oxide film to form a composite thin film of a metal element and a metal oxide on the surface of the basalt fiber.

[0020] As a further improvement of the present application, the concentration of the NaOH solution is 1-5 mol / L; the concentration of the dilute hydrochloric acid is 1-5 mol / L; and in the mixed solution, the molar ratio of dilute hydrochloric acid to dilute sulfuric acid is 1:1. As a further improvement of the present application, the thickness of the metal element film or the metal oxide film deposited on the surface of the basalt fiber is controlled by controlling the working time in the reaction chamber; in step S1, the method for cleaning the basalt fiber is to place the basalt fiber in an ethanol solution for ultrasonic treatment for 5-60 min.

[0021] As a further improvement of the present application, the structural film is preferably a composite film of different metal elements and metal oxides, or a composite film of metal elements and their metal oxides, and the loading method is specifically:

[0022] S21, under the condition that the working gas in the reaction chamber is argon, the metal element is used as the target material, and the metal element is bombarded to the surface of the basalt fiber under the action of the electric field to deposit and form a basalt fiber loaded with the metal element film;

[0023] S22, using argon as the working gas and oxygen as the reaction gas, and using the metal element as the target material, the metal atoms react with the oxygen atoms to generate oxides under the action of the electric field, and continue to deposit on the basalt fiber loaded with the metal element film in step S21 to form a basalt fiber loaded with the structural film on the surface; the metal element and the metal element in step S21 are the same or different.

[0024] The beneficial effects of the present application are:

[0025] 1. The present application provides a color basalt fiber resistant to extreme high temperature, which comprises a basalt fiber and a structural film coated on the surface of the basalt fiber, the structural film comprising a metal element film and / or a metal oxide film, and the metal element film or the metal oxide film is combined with the basalt fiber and different film layers of the structural film in a chemical bonding manner. The present application loads the metal element film and / or the metal oxide film on the surface of the basalt fiber to form a structural stable flame-retardant nanocrystal on the surface of the basalt fiber, which endows the basalt fiber with the property of resisting extreme high temperature, and utilizes the difference in refractive index between the basalt fiber, the metal element and the metal oxide to make the basalt fiber appear different colors, thereby solving the problem that the basalt fiber cannot be colored and expanding the application field of the basalt fiber.

[0026] 2、The application first performs surface micro-etching on basalt fiber, selects appropriate micro-etching solution and time, increases the surface roughness of the basalt fiber on the basis of not damaging the mechanical properties of the basalt fiber, increases the contact between the metal element and the surface of the basalt fiber, activates the basalt fiber through plasma treatment, increases the active groups on the surface of the basalt fiber, makes the subsequent metal atoms coordinate with the basalt fiber, and increases the bonding force between the metal element film and the basalt fiber. In addition, when the composite film of the metal element and the metal oxide is loaded on the surface of the basalt fiber, the metal element film is first deposited by using the coordination of the metal atoms with the surface of the basalt fiber, oxygen is introduced, the oxygen molecules of the diatomic atoms are first contacted with the metal atoms on the surface of the metal element film, and the metal atoms of the target material are bombarded to the surface of the metal element film and chemically combined with the oxygen atoms on the surface, so that the interface bonding capacity is improved, more target metal atoms are directly generated into metal oxides by reacting with oxygen when moving freely in the reaction chamber, and the metal oxides are continuously deposited on the surface of the metal element film of the basalt fiber to form a metal oxide film with a nano-crystal structure. Through the preparation method of the application, the basalt fiber and the film, and different film layers of the composite film are combined by chemical bonds, and finally the structural film with strong interface bonding force, closely combined film layers, extreme high temperature resistance and different colors is obtained on the surface of the basalt fiber.

[0027] 3、The application also adjusts the thickness of the metal element film and / or the metal oxide film, so that the color of the basalt fiber changes continuously, and the color is bright and has high saturation. In addition, the structural film on the surface of the basalt fiber not only does not affect the original performance of the basalt fiber, such as the high-strength performance, but also improves the flame-retardant performance of the basalt fiber, so that the basalt fiber can resist extreme high temperature and can be applied to the fields of fire-fighting clothes, fireproof clothes, fire blankets and the like.

[0028] 4、The preparation method of the application is simple and easy to implement, and realizes the color development and extreme high temperature resistance of the basalt fiber. The method does not involve any chemical dyes or other harmful substances, is pollution-free to the environment, is green and environmentally friendly, and is suitable for industrial production. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 The electron microscope images of the surface and section of the extreme high temperature resistant colored basalt fiber prepared in Example 1.

[0030] Figure 2 The fabric image prepared by using the extreme high temperature resistant colored basalt fiber prepared in Example 1.

[0031] Figure 3 The fabric image prepared by using the extreme high temperature resistant colored basalt fiber prepared in Examples 2-7. DETAILED DESCRIPTION

[0032] In order to make the objects, technical solutions and advantages of the present application clearer, the following will describe the present application in detail with reference to the accompanying drawings and specific embodiments.

[0033] It should be noted here that, in order not to obscure the present application with unnecessary details, only the structures and / or processing steps closely related to the solutions of the present application are shown in the accompanying drawings, and other details not closely related to the present application are omitted.

[0034] It should also be noted that the terms "comprise", "contain" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements, but also includes other elements not explicitly listed or inherent to such a process, method, article or device.

[0035] The colored basalt fiber resistant to extremely high temperature comprises a basalt fiber and a structural film coated on the surface of the basalt fiber, the structural film comprises one of a metal element film, a metal oxide film, a composite film of different metal elements or metal oxides, and a composite film of a metal element and a metal oxide; the structural film and the basalt fiber, and different film layers of the structural film are combined in a chemical bonding manner. The present application loads a metal element film and / or a metal oxide film on the surface of the basalt fiber, adjusts the thickness ratio of the metal element film and / or the oxide film, forms a structural stable flame-retardant nanocrystal on the surface of the basalt fiber, does not affect the original performance of the basalt fiber, such as the high-strength performance, endows the basalt fiber with the resistance to extremely high temperature, and makes the basalt fiber applicable to the fields of firefighting clothes, fireproof clothes, and fire blankets.

[0036] In particular, when the structural film is a metal element film or a metal oxide film, the difference in refractive index between the metal element film or the metal oxide film and the basalt fiber is at least 0.17; when the structural film is a composite film, the difference in refractive index between different film layers in the composite film is at least 0.17; and the refractive index of the metal element film or the metal oxide film is greater than 1.76. In this way, the difference in refractive index between the basalt fiber and the structural film or between different film layers of the structural film is utilized to make the basalt fiber appear different colors, solve the problem that the basalt fiber cannot be colored, and expand the application field of the basalt fiber.

[0037] Preferably, the structural film is a composite film of a metal element and a metal oxide, the metal element in the metal element and the metal oxide being the same or different; the total thickness of the structural film is 10-300 nm; in the composite film, the thickness ratio of the film layer formed by the metal element to the film layer formed by the metal oxide is (1-6):(1-6). When the composite film between the metal element and the metal oxide is loaded on the surface of the basalt fiber, multiple refractive index differences are formed among the basalt fiber, the metal element and the metal oxide, so that the obtained colored basalt fiber produces a color with higher saturation and has better resistance to extreme high temperature.

[0038] Specifically, the material of the structural film is one or more of a group IIIA element, a group IVA element except carbon, a group IB element, a group IIB element, a group IIIB element, a group IVB element, a group VB element, a group VIB element, a group VIII element, or one or more of a metal oxide thereof.

[0039] More specifically, the group IIA element is Mg, the group IIIA element is Al or Ga, the group IVA element is Si, the group IB element is Ag, the group IIB element is Zn, the group IIIB element is Y or Ce, the group IVB element is Ti, Zr or Hf, the group VB element is V or Ta, the group VIB element is Mo or W, and the group VIII element is Co or Pt.

[0040] A method for preparing a colored basalt fiber resistant to extreme high temperature, comprising the following steps:

[0041] S1, placing the cleaned basalt fiber in a micro-etching solution and reacting for 10-60 min, and then placing it in a plasma cleaning machine for surface treatment for 2-10 min;

[0042] S2, loading a metal element film and / or a metal oxide film on the surface of the basalt fiber treated in step S1 to obtain a colored basalt fiber resistant to extreme high temperature; the metal element film or the metal oxide film and the basalt fiber, and different film layers in the composite film are combined in a chemical bonding manner to form a structural film on the surface of the basalt fiber, and the thickness of the structural film is 10-300 nm.

[0043] The method for preparing the colored basalt fiber resistant to extreme high temperature does not involve any chemical dyes or other harmful substances, has no pollution to the environment, is green and environmentally friendly, and is suitable for industrial production.

[0044] In particular, in step S1, the micro-etching solution comprises one of a NaOH solution, dilute hydrochloric acid, or a mixed solution of dilute hydrochloric acid and dilute sulfuric acid; the reaction time of micro-etching is 10-60 min, and the micro-etching solution is preferably a NaOH solution. By micro-etching the basalt fiber surface, selecting an appropriate micro-etching solution and time, the surface roughness of the basalt fiber is increased without damaging the mechanical properties of the basalt fiber itself, the contact between the metal element and the basalt fiber surface is increased, and the activity groups on the surface of the basalt fiber are increased by plasma treatment, so that the metal atoms and the basalt fiber are coordinated, and the bonding force between the metal element film and the basalt fiber is increased.

[0045] In some specific embodiments, the concentration of the NaOH solution is 1-5 mol / L; the concentration of the dilute hydrochloric acid is 1-5 mol / L; and in the mixed solution, the molar ratio of dilute hydrochloric acid to dilute sulfuric acid is 1:1.

[0046] In some specific embodiments, in step S1, the method for cleaning the basalt fiber is to place the basalt fiber in an ethanol solution and ultrasonically treat for 5-60 min.

[0047] Specifically, in step S2, the method for loading the structural film on the surface of the basalt fiber is specifically:

[0048] The method for loading the metal element film is to use a metal element as a target material under the condition that the working gas in the reaction chamber is argon, and the metal element is bombarded to the surface of the basalt fiber to deposit under the action of an electric field, so as to form a basalt fiber loaded with a metal element film;

[0049] The method for loading the metal oxide film is to use a metal element as a target material under the condition that argon is used as the working gas and oxygen is used as the reaction gas in the reaction chamber, and the metal atoms and oxygen atoms react to form an oxide under the action of an electric field, so as to form a basalt fiber loaded with a metal oxide film;

[0050] The method for loading the metal element film is combined with the method for loading the metal oxide film to form a composite film of the metal element and the metal oxide on the surface of the basalt fiber.

[0051] In particular, the structural film is preferably a composite film of a metal element and a metal oxide, wherein the metal elements in the metal element and the metal oxide are the same or different, and the loading method is specifically:

[0052] S21, under the condition that the working gas in the reaction chamber is argon, a metal element is used as a target material, and the metal element is bombarded to the surface of the basalt fiber to deposit under the action of an electric field, so as to form a basalt fiber loaded with a metal element film;

[0053] S22, under the action of an electric field, metal atoms and oxygen atoms react to generate oxides, and continue to deposit on the basalt fiber loaded with the metal single substance film in step S21 to form a basalt fiber with a surface-loaded structure film; the metal single substance and the metal single substance in step S21 are the same or different.

[0054] In the process of loading the composite thin film of the metal single substance and the metal oxide on the surface of the basalt fiber, the metal single substance film is first loaded on the surface of the basalt fiber by coordination of the metal atoms and the surface of the basalt fiber, and then oxygen is introduced to make the diatomic oxygen molecules first contact and react with the metal atoms on the surface of the metal single substance film. When the metal atoms of the target are bombarded to the surface of the sample, the metal atoms combine with the oxygen atoms on the surface by chemical bonds, thereby improving the interface bonding capacity. More target metal atoms move freely in the reaction chamber and directly react with oxygen to generate metal oxides, which continue to deposit on the surface of the basalt fiber to form a metal oxide film with a nanocrystalline structure. In this way, by the preparation method, the basalt fiber and the film, and the different film layers of the composite thin film are combined by chemical bonds, and finally a structure film with strong interface bonding force, closely combined film layers, extreme high temperature resistance, and different colors is obtained on the surface of the basalt fiber.

[0055] More specifically, in step S2, steps S21 and S22, the thickness of the metal single substance film and / or the metal oxide film deposited on the surface of the basalt fiber is controlled by controlling the working time. In this way, by adjusting the thickness between the metal single substance film and the metal oxide film on the surface of the basalt fiber, the color development of the basalt fiber is continuously changed, and the color is bright and has high saturation. In addition, the structure film on the surface of the basalt fiber not only does not affect its original performance, such as high strength performance, but also improves the flame retardant performance of the basalt fiber, so that it can resist extreme high temperature and improve the application performance of the basalt fiber.

[0056] It should be noted that in step S2, the method of loading the structure film on the surface of the basalt fiber can also be one of layer-by-layer self-assembly, spin-on atomic layer deposition, molecular layer deposition, multiphoton ionization, plasma-enhanced chemical vapor deposition, vacuum sputtering, electroplating, chemical plating, and chemical bonding.

[0057] Example 1

[0058] The present embodiment 1 provides a preparation method of a color basalt fiber resistant to extreme high temperature, comprising the following steps:

[0059] S1, the basalt fiber is ultrasonically cleaned in an ethanol solution for 40 min, the cleaned basalt fiber is placed in a NaOH solution for reaction for 30 min, and then is placed in a plasma cleaning machine for surface treatment for 3 min.

[0060] S2, load the basalt fiber surface treated in step S1 with metal element film and metal oxide film in sequence to obtain color basalt fiber resistant to extreme high temperature; the specific steps are as follows:

[0061] S21, place the basalt fiber on a substrate support at 60 revolutions per minute in a reaction chamber under the condition that argon is used as working gas, use metal Ag as target material, and bombard Ag to the surface of the basalt fiber to deposit under the action of electric field to form basalt fiber loaded with Ag element film; wherein the deposition time is 0.5 h, and the thickness of the Ag element film is 25 nm;

[0062] S22, use argon as working gas, introduce oxygen as reaction gas, use metal Ti as target material, and generate TiO2 by the reaction of Ti and oxygen atoms under the action of electric field, and continue to deposit on the basalt fiber loaded with Ag element film in step S21, the deposition time is 3 h, and the basalt fiber loaded with structural film with a total thickness of 175 nm on the surface is formed.

[0063] Please refer to Figure 1 Figure 1 shows the electron microscope images of the surface and cross section of the color basalt fiber resistant to extreme high temperature prepared in Example 1. As can be seen from the figure, the structural film with a certain thickness is successfully loaded on the surface of the basalt fiber by using the method.

[0064] Please refer to Figure 2 Figure 2 shows the fabric prepared by using the color basalt fiber resistant to extreme high temperature prepared in Example 1. As can be seen from Figure 2 the figure, the color is successfully generated on the surface of the basalt fiber by using the method, and the specific color is green.

[0065] Example 2

[0066] The preparation method of the color basalt fiber resistant to extreme high temperature provided in this embodiment is different from that in Example 1 in that the deposition time of steps S21 and S22 is controlled to be 0.5 h and 0.5 h respectively, so that the thickness of the Ag element film on the surface of the basalt fiber is 25 nm, and the thickness of the TiO2 structural film is 25 nm; the rest is substantially the same as that in Example 1, and will not be repeated here.

[0067] Example 3

[0068] The preparation method of the color basalt fiber resistant to extreme high temperature provided in this embodiment is different from that in Example 1 in that the deposition time of steps S21 and S22 is controlled to be 0.5 h and 1 h respectively, so that the thickness of the Ag element film on the surface of the basalt fiber is 25 nm, and the thickness of the TiO2 structural film is 50 nm; the rest is substantially the same as that in Example 1, and will not be repeated here.

[0069] Example 4

[0070] The present example provides a method for preparing a color basalt fiber resistant to extremely high temperature. Compared with Example 1, the difference is that the deposition time of steps S21 and S22 is controlled to be 0.5 h and 1.25 h respectively, so that the thickness of the elemental Ag film on the surface of the basalt fiber is 25 nm, and the thickness of the TiO2 structural film is 62 nm; the rest is substantially the same as Example 1, which is not repeated here.

[0071] Example 5

[0072] The present example provides a method for preparing a color basalt fiber resistant to extremely high temperature. Compared with Example 1, the difference is that the deposition time of steps S21 and S22 is controlled to be 0.5 h and 1.5 h respectively, so that the thickness of the elemental Ag film on the surface of the basalt fiber is 25 nm, and the thickness of the TiO2 structural film is 75 nm; the rest is substantially the same as Example 1, which is not repeated here.

[0073] Example 6

[0074] The present example provides a method for preparing a color basalt fiber resistant to extremely high temperature. Compared with Example 1, the difference is that the deposition time of steps S21 and S22 is controlled to be 0.5 h and 2 h respectively, so that the thickness of the elemental Ag film on the surface of the basalt fiber is 25 nm, and the thickness of the TiO2 structural film is 100 nm; the rest is substantially the same as Example 1, which is not repeated here.

[0075] Example 7

[0076] The present example provides a method for preparing a color basalt fiber resistant to extremely high temperature. Compared with Example 1, the difference is that the deposition time of steps S21 and S22 is controlled to be 0.5 h and 2.5 h respectively, so that the thickness of the elemental Ag film on the surface of the basalt fiber is 25 nm, and the thickness of the TiO2 structural film is 125 nm; the rest is substantially the same as Example 1, which is not repeated here.

[0077] Please refer to Figure 3 Fig. 1 is a diagram of a fabric prepared from the color basalt fiber resistant to extremely high temperature prepared by Examples 2-6. From Figure 3 It can be seen that by adjusting the thickness of the metal elemental film and / or metal oxide film on the surface of the basalt fiber, the color of the basalt fiber changes continuously, and the color is bright and high in saturation.

[0078] The basalt fibers prepared by Examples 2-7 were subjected to high temperature resistance performance and color comparison, wherein the high temperature resistance performance was represented by whether the basalt fiber was melted by the flame spray gun within the same time, and the results are shown in the following table.

[0079] Table 3 Performance characterization of basalt fibers prepared in Examples 2-7

[0080] Product name Color Fusing Example 2 Silver Yes Example 3 Yellow No Example 4 Purple No Example 5 Indigo No Example 6 Green No Example 7 Pink No

[0081] As shown in Table 3, with different deposition times, the thicknesses of the elemental metal film and / or the metal oxide film on the surface of the basalt fiber are different, which causes the color of the basalt fiber to change continuously and different colors to be produced; and with the increase in the deposition thickness, the number of flame-retardant crystals on the surface of the basalt fiber increases, which sharply increases the high-temperature resistance of the basalt fiber.

[0082] Example 8

[0083] Example 8 provides a method for preparing a high-temperature-resistant colored basalt fiber. Compared with Example 1, the difference is that the step S22 is not performed, and the obtained basalt fiber only carries an Ag film. The rest is substantially the same as Example 1, and is not repeated here.

[0084] Example 9

[0085] Example 9 provides a method for preparing a high-temperature-resistant colored basalt fiber. Compared with Example 1, the difference is that the step S21 is not performed, and a TiO2 film is directly loaded on the surface of the basalt fiber. The rest is substantially the same as Example 1, and is not repeated here.

[0086] The color change, color saturation, and high-temperature resistance of the basalt fibers prepared in Examples 1, 8, and 9 are compared. The high-temperature resistance is indicated by whether the flame gun melts the basalt fiber within the same time. The results are shown in the following table.

[0087] Table 1 Performance characterization of basalt fibers prepared in Examples 1, 8, and 9

[0088] Product name Color change Saturation Fusing Example 1 Yes High No Example 8 No - Yes Example 9 Yes Low No

[0089] As shown in Table 1, the basalt fiber in Example 1 can produce a high-saturation color and has excellent high-temperature resistance after the deposition of the elemental silver film and the TiO2 film. In Example 8, the deposition of the TiO2 film is not performed, the color on the surface of the basalt fiber does not change significantly, and the high-temperature resistance is poor. In Example 9, the TiO2 film is directly deposited to obtain a colored basalt fiber, but the saturation of the color is low.

[0090] In summary, the application provides a kind of color basalt fiber resistant to extreme high temperature and a preparation method thereof, comprising basalt fiber and structural film coated on the surface of the basalt fiber, the structural film comprising one of metal element film, metal oxide film, composite film of different metal elements or metal oxides, and composite film of metal element and metal oxide; the structural film and the basalt fiber, and different film layers of the structural film are combined by chemical bonding.The application first performs surface micro-etching on the basalt fiber to increase the surface roughness, increase the contact between the metal element and the surface of the basalt fiber, and activate the basalt fiber by plasma treatment to increase the bonding force between the metal element film and the basalt fiber.In addition, when loading the composite film on the surface of the basalt fiber, the application first loads the metal element film by using the coordination of metal atoms and the surface of the basalt fiber, then introduces oxygen, and uses the oxygen molecules of two atoms to contact and react with the metal atoms on the surface of the metal element film, so that the metal atoms of the target material are bombarded to the surface of the metal element and chemically bonded with the oxygen atoms on the surface, thereby improving the interface bonding capacity, and more target metal atoms react with oxygen to directly generate metal oxides when moving freely in the reaction chamber, and continue to deposit on the surface of the basalt fiber to form a metal oxide film with nanocrystalline structure.By the preparation method of the application, the basalt fiber and the film, and different film layers of the composite film are combined by chemical bonding, and finally a structural film with strong interface bonding force, tightly combined film layers, resistance to extreme high temperature, and different colors is obtained on the surface of the basalt fiber.The application loads the metal element film and / or metal oxide film on the surface of the basalt fiber to form a structural stable flame-retardant nanocrystal on the surface of the basalt fiber, endow the basalt fiber with resistance to extreme high temperature, and use the difference in refractive index between the basalt fiber and the film, and different film layers of the composite film to make the basalt fiber appear different colors, solve the problem of colorless basalt fiber, and expand the application field of basalt fiber.

[0091] The above examples are only used to illustrate the technical solutions of the application but not limit the application, and although the application has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solutions of the application can be modified or replaced equivalently without departing from the spirit and scope of the technical solutions of the application.

Claims

1. A colored basalt fiber resistant to extreme high temperatures, characterized in that, The invention includes basalt fibers and a structural membrane covering the surface of the basalt fibers. The structural membrane comprises a composite film of elemental metal and metal oxide, wherein the refractive index difference between different layers of the composite film is at least 0.

17. The structural membrane and the basalt fibers, as well as the different layers of the structural membrane, are chemically bonded together. The preparation method of the colored basalt fiber resistant to extreme high temperatures includes the following steps: S1. Place the cleaned basalt fiber in a micro-etching solution and react for 10-60 minutes. Then, place it in a plasma cleaner for surface treatment for 2-10 minutes. S2. Load the surface of the basalt fiber treated in step S1 with a metal element film and a metal oxide film to obtain colored basalt fiber resistant to extreme high temperature; the metal element film and the basalt fiber, as well as the different film layers in the composite film, are chemically bonded to form a structural film on the surface of the basalt fiber, and the thickness of the structural film is 10-300 nm. The specific method for loading the structural membrane onto the surface of basalt fibers is as follows: S21. Under the condition that the working gas in the reaction chamber is argon, a metal element is used as the target material and bombarded onto the surface of basalt fiber under the action of an electric field to form a basalt fiber loaded with a metal element film. S22. Using argon as the working gas, oxygen as the reaction gas, and a metallic element as the target material, under the action of an electric field, metal atoms react with oxygen atoms to generate oxides, which are then deposited onto the basalt fibers loaded with the metallic element film in step S21 to form a basalt fiber surface-loaded structural film; the metallic element in step S22 may be the same type or a different type of metallic element from the metallic element in step S21.

2. The colored basalt fiber resistant to extreme high temperatures according to claim 1, characterized in that, In the composite film, the thickness ratio of the film layer formed by the metal element to the film layer formed by the metal oxide is (1~6):(1~6).

3. The colored basalt fiber resistant to extreme high temperatures according to claim 1, characterized in that, The metallic element of the structural film is one or more of the following: Al or Ga from Group IIIA, Ag from Group IB, Zn from Group IIB, Y or Ce from Group IIIB, Ti, Zr or Hf from Group IVB, V or Ta from Group VB, Mo or W from Group VIB, and Co or Pt from Group VIII.

4. The colored basalt fiber resistant to extreme high temperatures according to claim 1, characterized in that, In step S1, the micro-etching solution includes one of NaOH solution, dilute hydrochloric acid, or a mixed solution of dilute hydrochloric acid and dilute sulfuric acid, and the micro-etching reaction time is 10 to 60 minutes.

5. The colored basalt fiber resistant to extreme high temperatures according to claim 4, characterized in that, The concentration of the NaOH solution is 1–5 mol / L; the concentration of the dilute hydrochloric acid is 1–5 mol / L; and the molar ratio of the dilute hydrochloric acid to the dilute sulfuric acid in the mixed solution is 1:

1.

6. The colored basalt fiber resistant to extreme high temperatures according to claim 1, characterized in that, The thickness of the metal elemental film or metal oxide film deposited on the surface of the basalt fiber is controlled by controlling the working time in the reaction chamber; in step S1, the basalt fiber is cleaned by ultrasonic treatment in an ethanol solution for 5 to 60 minutes.

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