CN115744962B - CuF (CuF)2And a method for preparing the same - Google Patents
CuF (CuF)2And a method for preparing the same Download PDFInfo
- Publication number
- CN115744962B CN115744962B CN202211506386.4A CN202211506386A CN115744962B CN 115744962 B CN115744962 B CN 115744962B CN 202211506386 A CN202211506386 A CN 202211506386A CN 115744962 B CN115744962 B CN 115744962B
- Authority
- CN
- China
- Prior art keywords
- reaction
- temperature
- cuf
- gas
- copper powder
- 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
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 95
- 239000007789 gas Substances 0.000 claims abstract description 62
- 229910016509 CuF 2 Inorganic materials 0.000 claims abstract description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 52
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 26
- 239000011261 inert gas Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 8
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 abstract description 6
- 239000011593 sulfur Substances 0.000 abstract description 6
- 238000006073 displacement reaction Methods 0.000 abstract description 3
- 238000007086 side reaction Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 7
- 239000010949 copper Substances 0.000 description 6
- 239000012265 solid product Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 229910021594 Copper(II) fluoride Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- GWFAVIIMQDUCRA-UHFFFAOYSA-L copper(ii) fluoride Chemical compound [F-].[F-].[Cu+2] GWFAVIIMQDUCRA-UHFFFAOYSA-L 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- -1 transition metal salt Chemical class 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a CuF 2 and a preparation method thereof, wherein the preparation method comprises the steps of firstly placing copper powder in a closed container, and introducing nitrogen or inert gas until the air in the reaction container is completely discharged; introducing SF 6 gas into the reaction vessel, and enabling the SF 6 gas and copper powder to react at high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃; after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing nitrogen or inert gas into the reaction system until the temperature of the reaction system is reduced to room temperature, so as to obtain the CuF 2. The method enables copper powder and SF 6 gas to directly undergo a displacement reaction at high temperature to generate CuF 2 and sulfur simple substance, and the sulfur simple substance is gasified to directly obtain CuF 2 with higher purity. The nitrogen or inert gas is adopted for protection before and after the reaction, thereby avoiding side reactions, ensuring the purity of the product and ensuring the safety of the reaction system.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and relates to CuF 2 and a preparation method thereof.
Background
With the rapid increase of the demand of lithium batteries, the CuF 2 can be used as an important lithium battery anode material due to the extremely high theoretical voltage, low price and low toxicity. The current method for preparing CuF 2 mainly comprises a liquid phase method, a solvothermal method, a vapor deposition method and the like, and is characterized in that the liquid phase method is used for preparing CuF 2, for example Liu Xiuming and the like, transition metal salt reacts with alkali to generate corresponding hydroxide, HF is added to react with the hydroxide to generate CuF 2, and finally redundant reactants are removed through evaporation to obtain CuF 2; thoralf Krahl et al reacted copper alkoxide with HF at-70℃to give CuF 2 using solvothermal method; brian Burrows et al directly oxidize copper electrodes with dry HF gas under energized conditions using a vapor deposition process to obtain CuF 2 deposited on the electrode surface. The existing preparation method of laboratory copper fluoride mainly uses highly toxic fluorine source HF high-activity fluoride as a fluorine source, not only has severe preparation conditions, but also uses highly toxic HF, the preparation method is dangerous, and meanwhile, the product is required to be subjected to post-treatment to improve the purity of the product, so that the operation is complicated and the laboratory requirement is high.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the CuF 2 and the preparation method thereof, thereby solving the technical problems of severe preparation conditions, complex operation and higher risk in the process of synthesizing the CuF 2 in the prior art.
The invention is realized by the following technical scheme:
a method for preparing CuF 2, comprising the steps of:
S1: placing copper powder in a closed container, and introducing nitrogen or inert gas until the air in the reaction container is completely discharged;
S2: introducing SF 6 gas into the reaction vessel, and enabling the SF 6 gas and copper powder to react at high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃;
s3: after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing nitrogen or inert gas into the reaction system until the temperature of the reaction system is reduced to room temperature, so as to obtain the CuF 2.
Preferably, the inert gas comprises one of helium or argon.
Preferably, in the step S1, the introducing speed of nitrogen or inert gas is 80-100 mL/min.
Preferably, in the step S1, the nitrogen or inert gas is introduced for 20 to 40 minutes.
Preferably, the copper powder has a purity of greater than 99%.
Preferably, in the step S2, the introducing speed of SF 6 gas is 40-50 mL/min.
Preferably, in the step S2, SF 6 gas is introduced into the reaction vessel, and after the flow rate of the gas flow is stabilized, the temperature programming treatment is performed on the reaction system, so that the SF 6 gas reacts with the copper powder at a high temperature.
Preferably, the temperature-raising rate of the program in the step S2 and the temperature-lowering rate in the step S3 are both 10 ℃/min.
Preferably, in the step S2, the reaction time of the high-temperature reaction is 50 to 80 minutes.
A CuF 2 is prepared by the method described above.
Compared with the prior art, the invention has the following beneficial technical effects:
The preparation method of CuF 2 enables copper powder and SF 6 gas to directly undergo a displacement reaction at high temperature, specifically, a copper simple substance and SF 6 are reacted to generate CuF 2 and a sulfur simple substance, meanwhile, the sulfur simple substance is gasified at the reaction temperature of 630-690 ℃, cuF 2.SF6 gas with higher purity is directly obtained without toxicity, the operation is safe, in addition, nitrogen or inert gas is adopted for protection in the early reaction stage and the later reaction stage, the occurrence of side reaction is effectively avoided, the purity of the product is ensured, and the reaction system is safer.
Furthermore, the introducing speed of nitrogen or inert gas is 80-100 mL/min, so that the air in the reaction system is more fully discharged.
Further, the nitrogen or inert gas is introduced for 20-40 min, so that the air in the reaction system is effectively discharged.
Further, the purity of the copper powder is more than 99%, and the purity of the product is effectively improved.
Further, the introducing speed of SF 6 gas is 40-50 mL/min, so that SF 6 gas and copper powder can be fully contacted and reacted.
Further, SF 6 gas is introduced into the reaction vessel, and after the flow speed of the gas flow is stable, the temperature programming treatment is carried out on the reaction system, so that the SF 6 gas and the copper powder react more fully.
Furthermore, the cooling rate in the step S3 is 10 ℃/min, so that the stability of the product structure is ensured.
In step S2, the reaction time of the high-temperature reaction is 50-80 min, so that SF 6 gas and copper powder fully react.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of the preparation of CuF 2 according to the present invention;
FIG. 2 is an X-ray diffraction (XRD) pattern of CuF 2 prepared in example 2 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of CuF 2 prepared in example 2 according to the present invention;
FIG. 4 is an EDS spectrum of CuF 2 prepared in example 2 of the present invention.
FIG. 5 is a TG-DSC of CuF 2 obtained in example 2 according to the present invention.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, the terms "comprising," including, "" containing, "" having, "or the like are intended to cover the meanings of" consisting of … … "and" consisting essentially of … …, "e.g.," a includes a "is intended to cover" a includes a and the other "and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
As shown in fig. 1, the present invention provides a preparation method of CuF 2, which includes the following steps:
s1: placing copper powder with purity of more than 99% in a closed container, and introducing nitrogen or inert gas until the air in the reaction container is completely discharged; wherein the inert gas comprises one of helium or argon.
S2: introducing SF 6 gas into the reaction vessel at a speed of 40-50 mL/min, and after the flow speed of the gas flow is stable, performing temperature programming treatment on the reaction system to enable SF 6 gas to react with copper powder at a high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃, and the reaction time of the high-temperature reaction is 50-80 min.
S3: after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing nitrogen or inert gas into the reaction system until the temperature of the reaction system is reduced to room temperature, so as to obtain the CuF 2. The temperature rise rate of the program in the step S2 and the temperature drop rate in the step S3 are 10 ℃/min.
According to the preparation method of CuF 2, the copper powder and SF 6 gas are subjected to a displacement reaction at a high temperature, specifically, a copper simple substance and SF 6 are subjected to a reaction to generate CuF 2 and a sulfur simple substance, and meanwhile, the sulfur simple substance is gasified at a reaction temperature of 630-690 ℃ to directly obtain CuF 2 with higher purity. In addition, the reaction is protected by adopting nitrogen or inert gas in the early reaction stage and the later reaction stage, so that side reactions are effectively avoided, the purity of the product is ensured, and the reaction system is safer. Compared with the existing CuF 2 preparation method, the method has the advantages of simple equipment, convenient operation, safe synthesis process, cheap and easily available raw materials, and is suitable for preparing copper fluoride in a large scale in a laboratory.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1
2G of copper powder (500 nm, purity 99.9%) is weighed into a ceramic crucible, nitrogen is continuously introduced into a tube furnace at a gas flow rate of 100mL/min until the air in the tube furnace is exhausted, SF 6 gas is slowly introduced into the tube furnace at a gas flow rate of 50mL/min, after the gas flow is stable, the temperature is raised to 600 ℃ at a temperature rising rate of 10 ℃/min, and the temperature is kept for 60min, so that the high-purity copper powder and SF 6 are fully subjected to thermal decomposition reaction. After the reaction is finished, nitrogen is continuously introduced as a protective gas, and after the temperature is reduced to room temperature, 2.7 g of white CuF 2 solid product is collected, and the yield is 79%.
Example 2
2G of copper powder (500 nm, purity 99.9%) is weighed into a ceramic crucible, nitrogen is continuously introduced into a tube furnace at a gas flow rate of 100mL/min until the air in the tube furnace is exhausted, SF 6 gas is slowly introduced into a reaction system at a flow rate of 50mL/min, after the gas flow is stable, the temperature is raised to 660 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 60min, so that the high-purity copper powder and SF 6 are subjected to thermal decomposition reaction fully. After the reaction is finished, nitrogen is continuously introduced as a protective gas, and after the temperature is reduced to room temperature, 3.0 g of white CuF 2 solid product is collected, and the yield is 86%.
The XRD pattern of CuF 2 prepared in this example is shown in fig. 2, and as can be seen from fig. 2, the diffraction peaks at angles of 2θ of 27.7 °, 33.7, 50.1 °, 57.2 ° and the like correspond to the diffraction peaks of (011), (110), (112) and (022) crystal planes (pdf#09-0136) of WS 2, respectively, when the solid product is subjected to phase composition analysis by XRD, and the prepared solid product is CuF 2.
The SEM picture of CuF 2 prepared in this example is shown in fig. 3, and as can be seen from fig. 3, cuF 2 prepared in the invention has uniform morphology distribution and good uniformity.
The EDS spectrum of CuF 2 prepared in this example is shown in FIG. 4, and as can be seen from FIG. 4, the ratio of Cu to F elements is close to 1:2, and the combination of XRD in FIG. 2 shows that the method of the invention successfully prepares CuF 2.
In order to study the generation mechanism of CuF 2 in the invention, a TG-DSC graph is obtained by using a comprehensive thermal analyzer (HCT-4), and the result is shown in FIG. 5. As can be seen from FIG. 5, when tungsten powder is heated from room temperature to room temperature at a heating rate of 5 ℃/min under SF 6 atmosphere, the weight of the material is increased within the range of 572-783 ℃, the weight increase rate is 38.3%, the maximum exothermic peak appears on the DSC curve at 653 ℃, the fluorination reaction is Cu (S) +SF 6(g)→CuF2 (S) +S (g), and the apparent activation energy is 56KJ/mol, so that the activation energy of the reaction is effectively reduced and the reaction is promoted by controlling the temperature.
Example 3
2G of copper powder (500 nm, purity 99.9%) is weighed into a ceramic crucible, helium is continuously introduced into a tube furnace at a gas flow rate of 100mL/min until the air in the tube furnace is exhausted, SF 6 gas is slowly introduced into the tube furnace at a speed of 50mL/min, after the gas flow is stable, the temperature is raised to 690 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 60min, so that the high-purity copper powder and SF 6 are subjected to thermal decomposition reaction fully. After the reaction is finished, helium is continuously introduced as a protective gas, and after the temperature is reduced to room temperature, 2.8 g of white CuF 2 solid product is collected, and the yield is 81%.
Example 4
The embodiment provides a preparation method of CuF 2, which comprises the following steps:
s1: placing copper powder with the purity of 99% in a closed container, and introducing nitrogen for 20min at 80mL/min to completely exhaust air in the reaction container;
S2: introducing SF 6 gas into the reaction vessel at a speed of 40mL/min, and after the flow speed of the gas flow is stable, performing temperature programming treatment on the reaction system, wherein the temperature programming speed is 10 ℃/min, so that the SF 6 gas reacts with copper powder at a high temperature; wherein the reaction temperature of the high-temperature reaction is 630 ℃, and the reaction time of the high-temperature reaction is 50min.
S3: after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing nitrogen into the reaction system until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, and the CuF 2 is prepared.
Example 5
The embodiment provides a preparation method of CuF 2, which comprises the following steps:
S1: placing copper powder with the purity of 99% in a closed container, and introducing nitrogen at the rate of 85mL/min for 25min to completely exhaust air in the reaction container;
S2: introducing SF 6 gas into the reaction vessel at the speed of 44mL/min, and after the flow speed of the gas flow is stable, performing temperature programming treatment on the reaction system, wherein the temperature programming speed is 10 ℃/min, so that the SF 6 gas reacts with copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 650 ℃, and the reaction time of the high-temperature reaction is 60min.
S3: after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing helium into the reaction system until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, and the CuF 2 is prepared.
Example 6
The embodiment provides a preparation method of CuF 2, which comprises the following steps:
S1: putting copper powder with the purity of 99.9% into a closed container, and introducing nitrogen for 35min at 90mL/min to completely discharge air in the reaction container;
S2: introducing SF 6 gas into the reaction vessel at the speed of 50mL/min, and after the flow speed of the gas flow is stable, performing temperature programming treatment on the reaction system, wherein the temperature programming speed is 10 ℃/min, so that the SF 6 gas reacts with copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 670 ℃, and the reaction time of the high-temperature reaction is 70min.
S3: after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing nitrogen into the reaction system until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, and the CuF 2 is prepared.
Example 7
The embodiment provides a preparation method of CuF 2, which comprises the following steps:
S1: placing copper powder with the purity of 99.9% in a closed container, and introducing argon gas at the concentration of 100mL/min for 40min to completely discharge air in the reaction container;
S2: introducing SF 6 gas into the reaction vessel at the speed of 50mL/min, and after the flow speed of the gas flow is stable, performing temperature programming treatment on the reaction system, wherein the temperature programming speed is 10 ℃/min, so that the SF 6 gas reacts with copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 690 ℃, and the reaction time of the high-temperature reaction is 80min.
S3: after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing argon into the reaction system until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, and the CuF 2 is prepared.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The preparation method of the CuF 2 is characterized by comprising the following steps of:
S1: placing copper powder in a closed container, and introducing nitrogen or inert gas until the air in the reaction container is completely discharged;
S2: introducing SF 6 gas into the reaction vessel, and enabling the SF 6 gas and copper powder to react at high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃;
s3: after the SF 6 gas and the copper powder react, cooling the reaction system, and simultaneously introducing nitrogen or inert gas into the reaction system until the temperature of the reaction system is reduced to room temperature to prepare the CuF 2;
The purity of the copper powder is more than 99%;
In the step S2, the introducing speed of SF 6 gas is 40-50 mL/min;
in the step S2, the reaction time of the high-temperature reaction is 50-80 min.
2. The method of claim 1, wherein the inert gas comprises one of helium or argon.
3. The method for preparing CuF 2 according to claim 1, wherein in step S1, the introducing speed of nitrogen or inert gas is 80-100 ml/min.
4. The method for preparing CuF 2 according to claim 1, wherein in step S1, the nitrogen or inert gas is introduced for 20 to 40 minutes.
5. The method for preparing CuF 2 according to claim 1, wherein in step S2, SF 6 gas is introduced into the reaction vessel, and after the flow rate of the gas flow is stabilized, the reaction system is subjected to temperature programming treatment, so that SF 6 gas reacts with copper powder at high temperature.
6. The method of claim 1, wherein the temperature increase rate of the process in step S2 and the temperature decrease rate in step S3 are both 10 ℃/min.
7. A CuF 2, obtainable by a process according to any one of claims 1 to 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211506386.4A CN115744962B (en) | 2022-11-28 | 2022-11-28 | CuF (CuF)2And a method for preparing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211506386.4A CN115744962B (en) | 2022-11-28 | 2022-11-28 | CuF (CuF)2And a method for preparing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115744962A CN115744962A (en) | 2023-03-07 |
| CN115744962B true CN115744962B (en) | 2024-05-24 |
Family
ID=85339753
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211506386.4A Active CN115744962B (en) | 2022-11-28 | 2022-11-28 | CuF (CuF)2And a method for preparing the same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115744962B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09285719A (en) * | 1996-04-23 | 1997-11-04 | Mitsubishi Electric Corp | Gaseous sulfur hexafluoride recovering and regenerating device and mobile recovering and regenerating device |
| JP2011155037A (en) * | 2010-01-26 | 2011-08-11 | Kyushu Institute Of Technology | Etching test method |
-
2022
- 2022-11-28 CN CN202211506386.4A patent/CN115744962B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09285719A (en) * | 1996-04-23 | 1997-11-04 | Mitsubishi Electric Corp | Gaseous sulfur hexafluoride recovering and regenerating device and mobile recovering and regenerating device |
| JP2011155037A (en) * | 2010-01-26 | 2011-08-11 | Kyushu Institute Of Technology | Etching test method |
Non-Patent Citations (1)
| Title |
|---|
| 稀土氧化物氟化反应过程的研究;颜世宏 等;稀土(第04期);16-19, 63 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115744962A (en) | 2023-03-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6720222B2 (en) | High-purity tungsten pentachloride and its synthesis method | |
| CN113135554A (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN112520703B (en) | Green preparation method of lithium sulfide | |
| US4753916A (en) | Metal oxides of molybdenum or molybdenum and tungsten | |
| JP6715985B2 (en) | Method for producing lithium sulfide | |
| US20210261411A1 (en) | Method of making anhydrous metal sulfide nanocrystals | |
| CN115744962B (en) | CuF (CuF)2And a method for preparing the same | |
| JP2021118030A (en) | Method for manufacturing sulfide-based solid electrolyte | |
| KR102131772B1 (en) | Titanium containing transition metal phosphide, catalyst for hydrogen evolution comprising the same, the preparation method thereof | |
| Christe et al. | Synthesis and characterization of tetrafluoroammonium hexafluorobismuthate and some properties of tetrafluoroammonium hexafluoroantimonate | |
| CN117142935A (en) | Preparation method of bis (acetylacetonate) tin | |
| CN112125283A (en) | Method for preparing lithium sulfide by solid-liquid mixing and heating | |
| CN112939053B (en) | Method for preparing transition metal oxide material containing oxygen vacancy | |
| US20220332578A1 (en) | Plasma-assisted synthesis for solid-state electrolyte materials | |
| CN107416896B (en) | Controllable method for preparing titanium oxide powder | |
| Bhat et al. | HNbWO6 and HTaWO6: novel oxides related to ReO3 formed by ion exchange of rutile-type LiNbWO6 and LiTaWO6 | |
| US4137297A (en) | Process for the production of titanium disulphide | |
| JP2023533811A (en) | Low-oxygen AlSc alloy powder and method for producing the same | |
| JPH1053414A (en) | Production of metal disulfide and formation of bimetal trisulfide by further treatment thereof | |
| WO2024070179A1 (en) | Method for producing tantalum nitride material, and tantalum nitride material | |
| CN114195103B (en) | Preparation method of alkali metal and alkaline earth metal sulfide | |
| JPH0393630A (en) | Production of copper molybdenum sulfide | |
| US3932597A (en) | Purification of alkali metal halides | |
| RU2778348C1 (en) | Method for obtaining high-purity anhydrous lithium molybdate | |
| JPH0442802A (en) | Production of high-purity metal fluoride |
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 |