A method for preparing high-density one-dimensional selenium-doped copper telluride chains

Abstract

This invention relates to a method for preparing high-density one-dimensional selenium-doped copper telluride chains, belonging to the field of nanomaterials technology. The method involves preparing a copper single-crystal substrate; evaporating and depositing tellurium powder onto the copper single-crystal substrate to obtain the substrate and a copper tellurium compound deposited on the substrate, controlling the temperature of the copper tellurium compound and the copper single-crystal substrate at 25–30°C during the deposition process; subjecting the substrate and the deposited copper tellurium compound to a first heating and holding treatment at the growth temperature; then evaporating and depositing selenium powder onto the substrate and the copper tellurium deposit to obtain a selenium-doped copper telluride deposit and the substrate, controlling the temperature of the substrate and the deposit at 25–30°C during the deposition process; and subjecting the obtained selenium-doped copper telluride deposit and the substrate to a second heating and holding treatment at the growth temperature to obtain high-density one-dimensional selenium-doped copper telluride chains. The one-dimensional selenium-doped copper telluride chains prepared by this invention have a width of less than 1 nanometer, a length of more than 50 nanometers, and all chains are uniformly oriented.

Description

Technical Field

[0001] This invention relates to a method for preparing high-density one-dimensional selenium-doped copper telluride chains, belonging to the field of nanomaterials technology. Background Technology

[0002] In recent years, transition metal sulfides have been extensively studied as electrocatalysts and photocatalysts in the hydrogen evolution reaction, making them crucial in industrial decarbonization processes. Furthermore, transition metal chalcogenides can be used as materials in solar cells for hydrogen energy conversion. Copper telluride, in particular, is of great significance as the back contact in CdTe / CdS photovoltaic cells because it has the potential to increase the conductivity at the absorber contact interface. Generally, precise knowledge of the properties and atomic arrangement of so-called active sites is essential for any catalytic reaction. Based on this structural information, it is necessary to understand the atomic-scale morphology of the material and the physicochemical properties of the active sites.

[0003] However, for copper tellurium compounds, according to previous literature, their surface morphology is closely related to the amount of tellurium added, and multiple structural phases often coexist on the surface. If the surface is modulated so that one phase is predominant, subsequent experimental methods can be designed based on the morphology.

[0004] Patent application number 2021111297628 discloses a method for preparing high-density nanoscale monolayer molybdenum dioxide islands. The method involves selecting a silver single crystal as a substrate, sequentially depositing selenium powder and molybdenum metal atoms onto the substrate surface, then annealing the sample after heating it to the growth temperature, thereby obtaining nanoscale monolayer molybdenum diselenide islands on the sample surface. Furthermore, by increasing the deposition time of selenium powder and molybdenum metal atoms, high-density nanoscale monolayer molybdenum diselenide islands can be obtained. However, this patent application produces a molybdenum dioxide island product, not the copper tellurium compound of this invention. Summary of the Invention

[0005] To address the problems and shortcomings of the existing technology, this invention provides a method for preparing high-density one-dimensional selenium-doped copper telluride chains. This invention utilizes the strategy that both tellurium powder and selenium powder will chemically react with a copper substrate to form compounds. Tellurium powder is deposited onto the surface of the copper substrate to obtain a sample with copper tellurium compounds and tellurium atoms on the copper substrate. The sample is heated to a growth temperature and then annealed. Selenium powder is then deposited onto the sample surface, and the sample is heated to a growth temperature and annealed again, ultimately yielding a high-density one-dimensional selenium-doped copper telluride chain product.

[0006] A method for preparing high-density one-dimensional selenium-doped copper telluride chains, the specific steps of which include:

[0007] Step 1: Prepare a copper single-crystal substrate;

[0008] Step 2: The tellurium powder is evaporated and deposited onto the copper single crystal substrate of Step 1 to obtain the substrate and the copper tellurium compound deposited on the substrate. The temperature of the copper tellurium compound on the substrate and the copper single crystal substrate is controlled at 25-30℃ during the deposition process.

[0009] Step 3: The substrate from Step 2 and the copper tellurium compound deposited on the substrate are subjected to a first heating and holding treatment to the growth temperature.

[0010] Step 4: Then, the selenium powder is evaporated and deposited onto the substrate and copper telluride deposit treated in Step 3 to obtain selenium-doped copper telluride deposit and substrate. The temperature of the substrate and deposit is controlled at 25-30℃ during the deposition process.

[0011] Step 5: The selenium-doped copper telluride deposit and the substrate obtained in Step 4 are subjected to a second heating to the growth temperature and held to obtain high-density one-dimensional selenium-doped copper telluride chains.

[0012] The preparation process of the copper single crystal substrate is as follows:

[0013] Step 1.1: In an ultra-high vacuum chamber, an argon ion sputtering process is performed on a copper substrate to obtain a copper substrate;

[0014] Step 1.2: Heat the copper substrate obtained in Step 1.1 to 450℃ and hold for 10-30 minutes to obtain a copper single crystal substrate.

[0015] In step 2, the tellurium powder evaporation temperature is 190℃~195℃, and the deposition time is 25min~30min.

[0016] In steps 3 and 5, the growth temperature is 100–400℃, and the temperature is maintained for 30 minutes.

[0017] In step 4, the selenium powder evaporation temperature is 120℃~125℃, and the deposition time is 1min~2min.

[0018] The stoichiometric ratio of the above-mentioned tellurium powder to copper substrate to form copper tellurium compound is including but not limited to 1:1, and the stoichiometric ratio of selenium powder to substrate and copper tellurium deposit is including but not limited to 1:5.

[0019] The beneficial effects of this invention are:

[0020] (1) The present invention can prepare selenium-doped copper telluride chain products, which have a one-dimensional regular and ordered internal structure and high density.

[0021] (2) The high-density one-dimensional selenium-doped copper telluride chain product prepared by the present invention is a planar six-membered ring structure composed of copper atoms, tellurium atoms and selenium atoms;

[0022] (3) The one-dimensional selenium-doped copper telluride chains prepared by the present invention have a width of less than 1 nanometer, a length of more than 50 nanometers, and all chains are uniformly oriented. Attached Figure Description

[0023] Figure 1 This is a scanning tunneling microscope image of the high-density one-dimensional selenium-doped copper telluride chain prepared in Example 1 of the present invention.

[0024] Figure 2 These are scanning tunneling microscope atomic resolution images and cellular structure diagrams of the high-density one-dimensional selenium-doped copper telluride chains prepared in Example 1 of this invention. Figure 2 a) and periodic chart ( Figure 2 b);

[0025] Figure 3 These are scanning tunneling microscope images, computational simulation diagrams, and atomic model diagrams of the high-density one-dimensional selenium-doped copper telluride chains prepared in Example 1 of this invention. Detailed Implementation

[0026] The present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0027] Test instruments and equipment:

[0028] Cryogenic scanning tunneling microscope: purchased from Omicron GmbH, Germany.

[0029] K-cell molecular evaporation source: purchased from Omicron, Germany.

[0030] Argon ion gun: purchased from Omicron, Germany.

[0031] raw material:

[0032] Selenium powder: purchased from Sigma-Aldrich, purity 99.99%.

[0033] Tellurium powder: purchased from Sigma-Aldrich, purity 99.9%.

[0034] Copper single crystal: purchased from MaTecK, purity 99.999%.

[0035] Example 1

[0036] The specific steps of this method for preparing high-density one-dimensional selenium-doped copper telluride chains include:

[0037] Step 1: Preparation of copper single crystal substrate; The preparation process of copper single crystal substrate is as follows:

[0038] Step 1.1: In an ultra-high vacuum chamber, an argon ion sputtering process is performed on a copper substrate to obtain a copper substrate;

[0039] Step 1.2: Heat the copper substrate obtained in Step 1.1 to 450℃ and hold for 10 minutes to obtain a copper single crystal substrate;

[0040] Step 2: 500mg of tellurium powder was evaporated and deposited on the 50g copper single crystal substrate from Step 1 using a thermally resistive K-cell molecular evaporation source at an evaporation temperature of 195℃ to obtain the substrate and the copper tellurium compound deposited on the substrate. During the deposition process, the temperature of the copper tellurium compound on the substrate and the copper single crystal substrate was controlled at 30℃, and the deposition time was 30min.

[0041] Step 3: The substrate from Step 2 and the copper tellurium compound deposited on the substrate are subjected to a first heating and holding treatment at the growth temperature of 400℃ for 30 minutes.

[0042] Step 4: Then, 100 mg of selenium powder was evaporated and deposited on the 50 g substrate and copper telluride deposit treated in Step 3 at an evaporation temperature of 125 °C using a thermally resistive K-cell molecular evaporation source to obtain selenium-doped copper telluride deposit and substrate. The temperature of the substrate and deposit was controlled at 30 °C during the deposition process, and the deposition time was 2 min.

[0043] Step 5: The selenium-doped copper telluride deposit and the substrate obtained in Step 4 are subjected to a second heating to the growth temperature and held for 30 minutes to obtain high-density one-dimensional selenium-doped copper telluride chains; the growth temperature is 400℃ and the holding time is 30 minutes.

[0044] The high-density one-dimensional selenium-doped copper telluride chain obtained in this embodiment is shown in the scanning tunneling microscope image. Figure 1 As shown, from Figure 1 It can be seen that the product of this invention is a high-density one-dimensional selenium-doped copper telluride chain.

[0045] The high-density one-dimensional selenium-doped copper telluride chain obtained in this embodiment is shown in the scanning tunneling microscope atomic resolution image and unit cell structure diagram. Figure 2 a) and periodic chart ( Figure 2 b), from Figure 2 As can be seen from (a) and (b), the major axis a = 1.31 nm and the minor axis b = 0.44 nm of the high-density one-dimensional selenium-doped copper telluride unit cell are both 1.31 nm and 0.44 nm respectively.

[0046] The high-density one-dimensional selenium-doped copper telluride chain prepared in Example 1 is shown in the scanning tunneling microscope image, computational simulation diagram, and atomic model diagram. Figure 3 As shown, from Figure 3 This can directly and effectively prove that the one-dimensional, regular, ordered, high-density selenium-doped copper telluride chain prepared by the preparation method of the embodiments of the present invention is a planar six-membered ring structure composed of copper atoms, tellurium atoms, and selenium atoms.

[0047] Example 2

[0048] The specific steps of this method for preparing high-density one-dimensional selenium-doped copper telluride chains include:

[0049] Step 1: Preparation of copper single crystal substrate; The preparation process of copper single crystal substrate is as follows:

[0050] Step 1.1: In an ultra-high vacuum chamber, an argon ion sputtering process is performed on a copper substrate to obtain a copper substrate;

[0051] Step 1.2: Heat the copper substrate obtained in Step 1.1 to 450℃ and hold for 30 minutes to obtain a copper single crystal substrate;

[0052] Step 2: 500mg of tellurium powder was evaporated and deposited on the 50g copper single crystal substrate from Step 1 using a thermally resistive K-cell molecular evaporation source at an evaporation temperature of 190℃ to obtain the substrate and the copper tellurium compound deposited on the substrate. During the deposition process, the temperature of the copper tellurium compound on the substrate and the copper single crystal substrate was controlled at 25℃ and the deposition time was 25min.

[0053] Step 3: The substrate from Step 2 and the copper tellurium compound deposited on the substrate are subjected to a first heating and holding treatment at 100°C for 30 minutes.

[0054] Step 4: Then, 100 mg of selenium powder was evaporated and deposited on the 50 g substrate and copper telluride deposit treated in Step 3 at an evaporation temperature of 120 °C using a thermally resistive K-cell molecular evaporation source to obtain selenium-doped copper telluride deposit and substrate. The temperature of the substrate and deposit was controlled at 25 °C during the deposition process, and the deposition time was 1 min.

[0055] Step 5: The selenium-doped copper telluride deposit and the substrate obtained in Step 4 are subjected to a second heating to the growth temperature and held for 30 minutes to obtain high-density one-dimensional selenium-doped copper telluride chains; the growth temperature is 100℃ and the holding time is 30 minutes.

[0056] Example 3

[0057] The specific steps of this method for preparing high-density one-dimensional selenium-doped copper telluride chains include:

[0058] Step 1: Preparation of copper single crystal substrate; The preparation process of copper single crystal substrate is as follows:

[0059] Step 1.1: In an ultra-high vacuum chamber, an argon ion sputtering process is performed on a copper substrate to obtain a copper substrate;

[0060] Step 1.2: Heat the copper substrate obtained in Step 1.1 to 450℃ and hold for 25 minutes to obtain a copper single crystal substrate;

[0061] Step 2: 500mg of tellurium powder was evaporated and deposited at a thermal resistance K-cell molecular evaporation source at an evaporation temperature of 192℃ onto the 50g copper single crystal substrate from Step 1 to obtain the substrate and the copper tellurium compound deposited on the substrate. The temperature of the copper tellurium compound on the substrate and the copper single crystal substrate was controlled at 28℃ during the deposition process, and the deposition time was 28min.

[0062] Step 3: The substrate from Step 2 and the copper tellurium compound deposited on the substrate are subjected to a first heating and holding treatment at the growth temperature of 300℃ for 30 minutes.

[0063] Step 4: Then, 100 mg of selenium powder was evaporated and deposited on the 50 g substrate and copper telluride deposit treated in Step 3 at an evaporation temperature of 122 °C using a thermally resistive K-cell molecular evaporation source to obtain selenium-doped copper telluride deposit and substrate. The temperature of the substrate and deposit was controlled at 28 °C during the deposition process, and the deposition time was 1 min.

[0064] Step 5: The selenium-doped copper telluride deposit and the substrate obtained in Step 4 are subjected to a second heating to the growth temperature and held for 30 minutes to obtain high-density one-dimensional selenium-doped copper telluride chains.

[0065] The specific embodiments of the present invention have been described in detail above with reference to the accompanying drawings. However, the present invention is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the spirit of the present invention.

Claims

1. A method for preparing a high-density one-dimensional selenium-doped copper telluride chain, characterized in that... The specific steps include: Step 1: Prepare a copper single-crystal substrate; Step 2: The tellurium powder is evaporated and deposited onto the copper single crystal substrate of Step 1 to obtain the substrate and the copper tellurium compound deposited on the substrate. The temperature of the copper tellurium compound on the substrate and the copper single crystal substrate is controlled at 25~30℃ during the deposition process. Step 3: The substrate from Step 2 and the copper tellurium compound deposited on the substrate are subjected to a first heating and holding treatment to the growth temperature. Step 4: Then, the selenium powder is evaporated and deposited on the substrate and copper telluride deposit treated in Step 3 to obtain selenium-doped copper telluride deposit and substrate. The temperature of the substrate and deposit is controlled at 25~30℃ during the deposition process. Step 5: The selenium-doped copper telluride deposit and the substrate obtained in Step 4 are subjected to a second heating to the growth temperature and held to obtain high-density one-dimensional selenium-doped copper telluride chains. In step 2, the tellurium powder evaporation temperature is 190℃~195℃, and the deposition time is 25min~30min; In steps 3 and 5, the growth temperature is 100~400℃, and the temperature is maintained for 30 minutes.

2. The method for preparing high-density one-dimensional selenium-doped copper telluride chains according to claim 1, characterized in that: The preparation process of the copper single crystal substrate is as follows: Step 1.1: In an ultra-high vacuum chamber, an argon ion sputtering process is performed on a copper substrate to obtain a copper substrate; Step 1.2: Heat the copper substrate obtained in Step 1.1 to 450℃ and hold for 10-30 minutes to obtain a copper single crystal substrate.

3. The method for preparing high-density one-dimensional selenium-doped copper telluride chains according to claim 1, characterized in that: In step 4, the selenium powder evaporation temperature is 120℃~125℃, and the deposition time is 1min~2min.

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