CN113856706B - Glass fiber cloth@Tb doped Cu x Te composite material and preparation method thereof - Google Patents
Glass fiber cloth@Tb doped Cu x Te composite material and preparation method thereof Download PDFInfo
- Publication number
- CN113856706B CN113856706B CN202111300240.XA CN202111300240A CN113856706B CN 113856706 B CN113856706 B CN 113856706B CN 202111300240 A CN202111300240 A CN 202111300240A CN 113856706 B CN113856706 B CN 113856706B
- Authority
- CN
- China
- Prior art keywords
- doped
- glass fiber
- fiber cloth
- composite material
- mixed solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000003365 glass fiber Substances 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 239000004744 fabric Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000010949 copper Substances 0.000 claims abstract description 56
- 239000011259 mixed solution Substances 0.000 claims abstract description 41
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 26
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 21
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 21
- ULJUVCOAZNLCJZ-UHFFFAOYSA-K trichloroterbium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Tb+3] ULJUVCOAZNLCJZ-UHFFFAOYSA-K 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 abstract 1
- 229960001484 edetic acid Drugs 0.000 description 18
- 239000000463 material Substances 0.000 description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 4
- 229910052771 Terbium Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011011 black crystal Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical group FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 150000004772 tellurides Chemical class 0.000 description 1
- SITVSCPRJNYAGV-UHFFFAOYSA-L tellurite Chemical compound [O-][Te]([O-])=O SITVSCPRJNYAGV-UHFFFAOYSA-L 0.000 description 1
- YJVUGDIORBKPLC-UHFFFAOYSA-N terbium(3+);trinitrate Chemical compound [Tb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YJVUGDIORBKPLC-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0576—Tellurium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemically Coating (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The application relates to a glass fiber cloth@Tb doped Cu x The Te composite material and the preparation method thereof comprise the following steps: a. dissolving sodium tellurite in a mixed solution of glycerol and water, and stirring to form a sodium tellurite solution; b. sequentially adding a certain amount of ethylenediamine tetraacetic acid, terbium chloride hexahydrate and anhydrous copper sulfate into the sodium tellurite solution, and stirring for a certain time to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, placing the reaction kettle into a constant temperature box, reacting for a certain time at a constant temperature, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material. The preparation method has simple preparation process, and the glass fiber cloth@Tb doped Cu with large specific surface area and uniform dispersion is obtained by a one-step method x Te composite material.
Description
Technical Field
The application relates to a glass fiber cloth@Tb doped Cu x A preparation method of Te composite material.
Background
Telluride has a wide range of physical and chemical properties, some of which exhibit metallic properties, in addition to being salt-like compounds, while others exhibit stronger covalent properties. The literature reports that a large number of tellurium-rich telluride compounds all have an anionic structure of Te-Te bonds. Wherein Cu is x Te is a black crystal powder which is stable in air at room temperature, is an important inorganic material for storing tellurium and copper resources, and is a binary compoundHas Cu x Te,Cu 2 Te,Cu x Te 2 ,Cu 3 Te 2 ,Cu 7 Te 4 Cu of non-stoichiometric composition 2-x Te, and the like. The copper telluride material has wide application prospect in solar cells, lasers, infrared detectors and superconducting materials, and is suitable for the current energy-saving and environment-friendly theme. The copper telluride nano material has important application prospect due to the unique micro-morphology and nano-performance and the special physicochemical optical characteristics displayed by the copper telluride nano material.
Although Cu is x The research on Te preparation has been greatly advanced, but Cu is present x The preparation method of Te is complex and the performance of Te is not high. To further improve the properties, it is generally possible to modify them by means of doping. The rare earth is called as industrial gold, and has excellent physical properties such as light and electromagnetic properties, can be combined with other materials to form novel materials with various properties and varieties, and the rare earth doping has greatly progressed in the aspect of development and research of functional composite materials, thereby being beneficial to improving the material properties.
In view of the above, the application prepares the glass fiber cloth @ Tb doped Cu by a one-step liquid phase method x Te composite material.
Disclosure of Invention
The application aims to provide the glass fiber cloth@Tb doped Cu which has the advantages of simple process, low cost, short reaction period, uniformity, large specific surface area and high performance x A preparation method of Te composite material.
Glass fiber cloth @ Tb doped Cu x The preparation method of the Te composite material comprises the following steps: a. dissolving sodium tellurite in a mixed solution of glycerol and water, and stirring to form a sodium tellurite solution; b. sequentially adding a certain amount of ethylenediamine tetraacetic acid, terbium chloride hexahydrate and anhydrous copper sulfate into the sodium tellurite solution, and stirring for a certain time to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for a certain time, placing the reaction kettle into a constant temperature box, reacting for a certain time at a constant temperature, naturally cooling to room temperature, cleaning, and drying to obtain the productObtaining the product glass fiber cloth @ Tb doped Cu x Te composite material. By the one-step method, the composite material with large specific surface and high performance can be simply and quickly prepared. And by doping Tb, cu is improved x Band gap of Te to increase Cu x Te structure stability and improved catalytic performance.
Further, the amount of sodium tellurite in the step a is 0.1-2.3g, the glycerol is 1-10ml, and the volume ratio of the glycerol to the water is 1:10-1:50. Wherein glycerol must be present and only in the proportions described above, a homogeneous composite material with a large specific surface can be obtained. If the material is changed into other alcohols or proportions, the surface of the obtained material is uneven or a burr-shaped structure cannot be obtained.
Further, the amount of ethylenediamine tetraacetic acid in step b is 0.02-0.5g.
Further, the terbium chloride hexahydrate in step b is present in an amount of 0.0001 to 0.02g.
Further, the amount of the anhydrous copper sulfate in the step b is 0.08-3.2g, and the stirring time is 10-60min. The amounts of copper sulfate and terbium chloride hexahydrate can be adjusted as desired. However, the addition of ethylenediamine tetraacetic acid is necessary, and only 0.02-0.5g of ethylenediamine tetraacetic acid is added, terbium can be uniformly doped into Cu x In Te materials, the surface of the Te material is in a burr-shaped structure, and if ethylenediamine tetraacetic acid or other proportions are not adopted, the uneven surface of the material cannot be obtained or the burr-shaped structure of the surface cannot be obtained.
Further, the ultrasonic time in the step c is 20-30min. After the ultrasonic wave is selected to be added into the reaction kettle, the mixed solution can be effectively contacted with the glass fiber cloth, so that the coating uniformity is improved.
Further, the constant temperature of the step c is 150-220 ℃ and the reaction time is 2-18h.
The application also comprises that the glass fiber cloth@Tb is doped with Cu x Te composite material, glass fiber cloth @ Tb doped Cu prepared by any one of the preparation methods x Te composite material.
Compared with the prior art, the application has the outstanding effects that:the glass fiber cloth@Tb of the application is doped with Cu x The preparation method of the Te composite material has the advantages of simple preparation process, low requirement on equipment and high controllable degree. The corresponding material can be obtained by selecting glycerol and water with a certain proportion and combining the combined synergistic effect of ethylene diamine tetraacetic acid with a certain proportion, specific terbium chloride and anhydrous copper sulfate, the material is uniformly coated, the surface is in a burr-shaped structure, the obtained material has larger specific surface area, and Cu can be improved by means of terbium doping x Te structure stability, cu is improved x Te photoelectric properties. In addition, the mixed solution can be effectively contacted with the glass fiber cloth by selecting the ultrasonic wave after the ultrasonic wave is added into the reaction kettle, so that the coating uniformity is improved, in addition, the problem of material aggregation can be effectively solved due to the addition of the glass fiber cloth, the formation of composite materials with uniform morphology and size can be facilitated, and the recycling is facilitated. Through reasonable process control, the glass fiber cloth@Tb Cu doping is realized x Preparation of Te composite material, glass fiber cloth @ Tb doped with Cu x The Te composite material has uniform size, novel shape, better performance and wide application in the energy and environmental protection industries.
Drawings
FIG. 1 is a graph of Cu doped with glass cloth @ Tb prepared in example 1 x SEM photograph of Te composite.
FIG. 2 is a graph of Cu doped with glass cloth @ Tb prepared in example 1 x SEM magnified photograph of Te composite.
Detailed Description
The present application will be further illustrated with reference to the following specific examples, but is not limited thereto.
Example 1
Glass fiber cloth @ Tb doped Cu x The preparation method of the Te composite material comprises the following specific steps: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into fourPlacing the reaction kettle in a fluoroethylene reaction kettle for ultrasonic treatment for 25min, placing the reaction kettle in an incubator for reaction for 12h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
The attached figures 1-2 are glass fiber cloth @ Tb doped Cu prepared by the method x SEM pictures of Te composite materials show that the glass fiber cloth@Tb doped Cu is successfully prepared x Te composite material with uniform size and uniform surface coating, wherein the surface of the material is of a burr-shaped structure, and Tb coated on the surface of glass fiber cloth is doped with Cu x The Te composite material is in a burr assembly layer structure, has a larger specific surface, is beneficial to later adsorption of other materials, and is beneficial to catalysis and other applications; the doping of Tb modifies the material better than the doping of Cu without Tb x Te has better photoelectric property, and can further improve the specific surface by means of glass fiber cloth to avoid aggregation.
Comparative example 1, which differs from example 1 in that no glycerol was added in step a, and in the same manner as in example 1, tb was doped with Cu x The Te composite cannot be coated on glass fiber cloth.
Comparative example 2, which differs from example 1 in that ethylenediamine tetraacetic acid was not added in step b, and otherwise is the same as in example 1, and as a result Tb was doped with Cu x The Te composite material is unevenly coated on the surface and is not in a burr-shaped structure.
Comparative example 3, which differs from example 1 in that step c does not involve an ultrasonic step, otherwise is the same as example 1, and as a result Tb is doped with Cu x The Te composite material is unevenly coated on the surface.
Comparative example 4, which differs from example 1 in that terbium chloride, anhydrous copper sulfate in step c are exchanged for other kinds of salts such as terbium nitrate, copper chloride, etc., otherwise identical to example 1, and as a result Tb is doped with Cu x The Te composite material is unevenly coated on the surface and is not in a burr-shaped structure. This is because the chloride in terbium chloride and the sulfate in anhydrous copper sulfate cooperate with each other, thereby further improving the surface morphology of the material.
Example 2
This example differs from example 1 in that the amount of sodium tellurite was changed to 0.444g, and otherwise the same as example 1, specifically as follows: a. dissolving 0.444g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box for reaction for 12h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Example 3
This example differs from example 1 in that the amount of anhydrous copper sulfate was changed to 0.32g, and otherwise the same as example 1 is as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.32g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box for reaction for 12h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Example 4
This example differs from example 1 in that the stirring time was changed to 60min, and otherwise the same as example 1, specifically as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 60min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box, reacting for 12h at 180 ℃, and naturallyCooling to room temperature, cleaning, drying to obtain the product glass fiber cloth @ Tb doped with Cu x Te composite material.
Example 5
This example differs from example 1 in that the amount of ethylenediamine tetraacetic acid was changed to 0.4g, and otherwise the same as in example 1, specifically as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.4g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box for reaction for 12h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Example 6
This example differs from example 1 in that the reaction temperature was changed to 200 ℃, and otherwise the same as example 1, specifically as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and the glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box, reacting for 12h at 200 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Example 7
This example differs from example 1 in that the reaction time was changed to 18h, otherwise the same as example 1, specifically as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. will be spentAdding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box, reacting for 18h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Example 8
This example differs from example 1 in that the amount of terbium chloride hexahydrate was changed to 0.01g, and otherwise the same as example 1, specifically as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.01g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box for reaction for 12h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Example 9
This example differs from example 1 in that the amounts of glycerol and water were changed to 6ml and 94ml, respectively, and the other is the same as example 1, specifically as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 6ml of glycerol and 94ml of water, and stirring to form a sodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.16g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box for reaction for 12h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Example 10
This example differs from example 1 in that the amount of anhydrous copper sulfate was changed to 0.08g, and otherwise the same as example 1, specifically as follows: a. dissolving 0.222g of sodium tellurite in a mixed solution of 3ml of glycerol and 47ml of water, and stirring to formSodium tellurite solution; b. sequentially adding 0.2g of ethylenediamine tetraacetic acid, 0.005g of terbium chloride hexahydrate and 0.08g of anhydrous copper sulfate into the sodium tellurite solution, and stirring for 30min to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for 25min, placing the reaction kettle into a constant temperature box for reaction for 12h at 180 ℃, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material.
Claims (6)
1. Glass fiber cloth@Tb doped Cu x The preparation method of the Te composite material is characterized by comprising the following steps of: a. dissolving sodium tellurite in a mixed solution of glycerol and water, and stirring to form a sodium tellurite solution; b. sequentially adding a certain amount of ethylenediamine tetraacetic acid, terbium chloride hexahydrate and anhydrous copper sulfate into the sodium tellurite solution, and stirring for a certain time to form a mixed solution; c. adding the mixed solution and glass fiber cloth into a tetrafluoroethylene reaction kettle, carrying out ultrasonic treatment for a certain time, placing the reaction kettle into a constant temperature box, reacting for a certain time at a constant temperature, naturally cooling to room temperature, cleaning, and drying to obtain the glass fiber cloth@Tb doped Cu product x Te composite material;
the amount of sodium tellurite in the step a is 0.1-2.3g, the glycerol is 1-10ml, and the volume ratio of the glycerol to the water is 1:10-1:50; the amount of ethylenediamine tetraacetic acid in step b is 0.02-0.5g.
2. The glass cloth @ Tb doped Cu of claim 1 x A process for the preparation of a Te composite, characterized in that in step b the amount of terbium chloride hexahydrate is between 0.0001 and 0.02g.
3. The glass cloth @ Tb doped Cu of claim 1 x The preparation method of the Te composite material is characterized in that the anhydrous copper sulfate in the step b is 0.08-3.2g, and the stirring time is 10-60min.
4. As claimed in1 @ Tb doped with Cu x The preparation method of the Te composite material is characterized in that the constant temperature in the step c is 150-220 ℃ and the reaction time is 2-18h.
5. The glass cloth @ Tb doped Cu of claim 1 x The preparation method of the Te composite material is characterized in that the ultrasonic time in the step c is 20-30min.
6. Glass fiber cloth@Tb doped Cu x Te composite material characterized in that glass fiber cloth @ Tb doped with Cu prepared by the method of any one of the above claims 1-5 x Te composite material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111300240.XA CN113856706B (en) | 2021-11-04 | 2021-11-04 | Glass fiber cloth@Tb doped Cu x Te composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111300240.XA CN113856706B (en) | 2021-11-04 | 2021-11-04 | Glass fiber cloth@Tb doped Cu x Te composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113856706A CN113856706A (en) | 2021-12-31 |
| CN113856706B true CN113856706B (en) | 2023-09-05 |
Family
ID=78986998
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111300240.XA Active CN113856706B (en) | 2021-11-04 | 2021-11-04 | Glass fiber cloth@Tb doped Cu x Te composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113856706B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101395247A (en) * | 2006-01-06 | 2009-03-25 | 新加坡国立大学 | Method of preparing nano-structured material(s) and uses thereof |
| CN109999867A (en) * | 2019-04-28 | 2019-07-12 | 浙江理工大学 | A kind of flexible carbon fibre cloth@BiOCl@Ag3PO4Optic catalytic composite material and preparation method thereof |
| CN111389418A (en) * | 2020-04-30 | 2020-07-10 | 浙江理工大学 | Flexible carbon fiber cloth @ Cu2O@SnS2Composite material, preparation method and application |
| CN111905687A (en) * | 2019-05-08 | 2020-11-10 | 浙江理工大学 | Flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material and preparation method thereof |
| CN111905689A (en) * | 2019-05-08 | 2020-11-10 | 浙江理工大学 | Flexible glass fiber cloth @ FeZn double-hydroxide adsorbing material and preparation method thereof |
-
2021
- 2021-11-04 CN CN202111300240.XA patent/CN113856706B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101395247A (en) * | 2006-01-06 | 2009-03-25 | 新加坡国立大学 | Method of preparing nano-structured material(s) and uses thereof |
| CN109999867A (en) * | 2019-04-28 | 2019-07-12 | 浙江理工大学 | A kind of flexible carbon fibre cloth@BiOCl@Ag3PO4Optic catalytic composite material and preparation method thereof |
| CN111905687A (en) * | 2019-05-08 | 2020-11-10 | 浙江理工大学 | Flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material and preparation method thereof |
| CN111905689A (en) * | 2019-05-08 | 2020-11-10 | 浙江理工大学 | Flexible glass fiber cloth @ FeZn double-hydroxide adsorbing material and preparation method thereof |
| CN111389418A (en) * | 2020-04-30 | 2020-07-10 | 浙江理工大学 | Flexible carbon fiber cloth @ Cu2O@SnS2Composite material, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 水热法合成一维纳米材料的研究进展;周菊红;王涛;陈友存;张元广;;化学通报(07);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113856706A (en) | 2021-12-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112875755B (en) | Preparation method of bismuth tungstate nano powder | |
| CN111138294A (en) | Novel two-dimensional double perovskite BA4AgSbBr8Method for producing single crystal | |
| CN102285681A (en) | Low-temperature hydrothermal synthesis method of ZnO nano shuttle | |
| CN102079541B (en) | Method for preparing doping type hexagonal system nano ZnS at low temperature | |
| CN103920517A (en) | Composite visible light photocatalyst and its preparation method | |
| CN113856706B (en) | Glass fiber cloth@Tb doped Cu x Te composite material and preparation method thereof | |
| CN110104623A (en) | A kind of preparation method of the four phosphatization cobalt of rich phosphorus transition metal phosphide of different-shape | |
| CN107418560B (en) | Preparation method of efficient sulfur-doped zinc oxide nano material | |
| CN103342396B (en) | Method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material | |
| CN107841791B (en) | Preparation method of single crystal indium nanowire, product and application thereof | |
| CN113996317B (en) | Carbon fiber cloth @ Ni doped MnSe x Te 2-x Composite material and preparation method thereof | |
| Liu et al. | Synthesis of ZnGa2O4 octahedral crystallite by hydrothermal method with the aid of CTAB and its photocatalytic activity | |
| CN103318955B (en) | A kind of string-like TiO 2sphere material and preparation method thereof | |
| CN114011443B (en) | Carbon fiber cloth @ ZnTe x S 2-x @Ag 3 PO 4 Composite material and preparation method thereof | |
| CN100389073C (en) | Preparation method of dendroid barium tungstate nano crystal | |
| CN101476160B (en) | Ultrasonic aging synthesis for manganese doped zinc sulphide nanocrystalline | |
| CN111974420A (en) | MnFe2O4@MoxSn1-xS2Magnetic catalytic material and preparation method thereof | |
| CN104229758A (en) | Preparation method for large size ZnSe nanosheet | |
| CN102774879B (en) | Preparation method of dual-phase coexistence one-dimensional structure tin dioxide | |
| CN113620342B (en) | Shuttle-shaped silver bismuth disulfide nano material and preparation method thereof | |
| CN101805013A (en) | Synthesis method for grenade-shaped nanometer zinc oxide with low-temperature control | |
| CN110357166B (en) | Method for preparing nano chalcopyrite tetrahedral crystal under hydrothermal condition | |
| CN114887614A (en) | Preparation method of ZnO flexible film with high optical performance | |
| Zhang et al. | Hemispheric ordered porous Eu (TTA) 3 (TPPO) 2/ZnO fluorescence composites and its preparation method | |
| CN112357958A (en) | Cesium-containing lead-free halide double perovskite material Cs2NaBi1-xSnxCl6-xPreparation method of (1) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |