Method for preparing electrocatalyst by regulating and adsorbing hydrogen phosphide through crystal face of nickel oxide
By controlling the crystal plane of nickel oxide to prepare NixPy electrocatalysts, the defects of phosphine removal and nickel-based catalyst application in PVC production have been solved, achieving the dual goals of efficient electrocatalytic water splitting and environmentally friendly resource utilization.
Patent Information
- Application Number
- CN202511848620.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-09
- Publication Date
- 2026-02-10
AI Technical Summary
Existing technologies are insufficient to effectively remove highly toxic phosphine from crude acetylene gas during PVC production, leading to catalyst deactivation and environmental pollution. Furthermore, transition metal nickel-based electrocatalysts have limitations in the application of electrocatalytic hydrogen production.
NixPy electrocatalytic materials were prepared by synthesizing nickel oxide particles with specific exposed crystal faces using a solvothermal or hydrothermal method and then phosphating them in a phosphine atmosphere to control the nickel oxide crystal faces for phosphine adsorption.
While achieving efficient removal of phosphine, a high-performance electrocatalyst was prepared, which has the dual effect of environmental protection and resource utilization, and is suitable for the field of electrocatalytic water splitting to produce hydrogen.
Smart Images

Figure CN121493905A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of electrocatalytic material preparation technology, specifically to a method for preparing electrocatalysts by controlling the adsorption of phosphine through nickel oxide crystal planes. Background Technology
[0002] As an important chemical material, PVC is widely used in various industries such as construction, power transmission, automobile manufacturing, consumer electronics, packaging, and medical equipment, and market demand continues to grow. With increasingly tight domestic resource and energy constraints and increasingly stringent environmental regulations, the PVC industry is gradually shifting from scale expansion to quality improvement, and the demand for green, high-performance PVC products is becoming increasingly urgent.
[0003] The core raw material for PVC production is crude acetylene gas. When crude acetylene gas is generated under anaerobic conditions, it contains not only acetylene but also a large amount of highly toxic phosphine. Phosphine, typically present in concentrations of 450-1400 mg / Nm³ (approximately 296-929 ppm), poses multiple hazards: firstly, it deactivates catalysts in PVC production, directly reducing product quality; secondly, phosphine is highly toxic to organisms, posing a serious threat to the environment and human health, and also depletes atmospheric hydroxyl radicals, weakening the atmosphere's ability to degrade other greenhouse gases, indirectly exacerbating global warming. Therefore, removing phosphine from crude acetylene gas is a pressing issue for the PVC industry.
[0004] In the field of electrocatalytic hydrogen production, transition metal nickel-based electrocatalysts are widely used, but most nickel-based catalysts have inherent defects that hinder large-scale application. Transition metal phosphides are considered one of the most promising alternatives to platinum and platinum-based catalysts, with nickel-based phosphides exhibiting excellent catalytic performance in both the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER). Morphological engineering can optimize the catalytic activity of metals and metal oxides by controlling factors such as crystal facets, surface free energy, and surface vacancies, achieving efficient charge transfer and water splitting reactions. Currently, morphology-controllable copper, cobalt, and manganese oxides have been extensively studied, but research on morphology control of nickel oxide remains relatively scarce.
[0005] Therefore, it is necessary to provide a method for preparing electrocatalysts by controlling the adsorption of phosphine through nickel oxide crystal planes. Summary of the Invention
[0006] The purpose of this invention is to provide a method for preparing electrocatalysts by controlling the adsorption of phosphine through nickel oxide crystal planes. This method can efficiently remove phosphine and simultaneously prepare high-performance electrocatalytic materials, thereby achieving the dual goals of environmental protection and resource utilization.
[0007] To achieve the above objectives, the present invention adopts the following technical solution:
[0008] A method for preparing an electrocatalyst by controlling the adsorption of phosphine by nickel oxide crystal facets involves using a nickel source as raw material to synthesize morphology-controllable nickel oxide particles with specific exposed crystal facets via a solvothermal or hydrothermal method. The nickel oxide particles are then heat-treated to obtain a precursor, which is subsequently subjected to phosphine treatment in a phosphine atmosphere to finally prepare a Ni-containing electrocatalyst. x P y Electrocatalytic materials; wherein the specific crystal planes include (111) crystal planes and (110) crystal planes.
[0009] Furthermore, the nickel source is nickel nitrate, specifically... The morphology-controllable nickel oxide particles include octahedral nickel oxide, hexahedral nickel oxide and ring-shaped nickel oxide, with the octahedral nickel oxide exposing the (111) crystal plane and the hexahedral nickel oxide exposing the (110) crystal plane.
[0010] Furthermore, the preparation of the octahedral nickel oxide includes the following steps:
[0011] (1) Weigh according to proportion ,Will It dissolves completely in 40 mL of anhydrous ethanol to form a homogeneous solution;
[0012] (2) Transfer the homogeneous solution obtained in step (1) into a hydrothermal reactor, seal the reactor and place it in a temperature control device, and perform a hydrothermal reaction at 110°C for 8 hours. After the reaction is completed, a dark green suspension is obtained.
[0013] (3) The dark green suspension obtained in step (2) is centrifuged to separate the solid product. The solid product is then placed in a vacuum oven to dry, and octahedral nickel oxide precursor powder is obtained.
[0014] (4) The precursor powder obtained in step (3) is placed in a tube furnace and heat-treated at 400°C for 2 hours in an air atmosphere. After heat treatment, the product is crushed and sieved to obtain octahedral nickel oxide precursor.
[0015] Furthermore, the preparation of the hexahedral nickel oxide includes the following steps:
[0016] (1) Weigh according to proportion and NaOH, and Dissolve them together in 40 mL of distilled water and stir until completely dissolved to form a homogeneous solution;
[0017] (2) Transfer the homogeneous solution obtained in step (1) into a hydrothermal reactor, seal the reactor and place it in a temperature control device, and perform a hydrothermal reaction at 180°C for 5 hours. After the reaction is completed, a dark green suspension is obtained.
[0018] (3) The dark green suspension obtained in step (2) was centrifuged and separated. The centrifugation speed was controlled at 7000 rpm and the centrifugation time was 10 minutes. The solid product was collected.
[0019] (4) The solid product obtained in step (3) is placed in a vacuum oven at 60°C and dried overnight to obtain hexahedral nickel oxide precursor powder;
[0020] (5) The precursor powder obtained in step (4) is placed in a tube furnace and heat-treated at 500°C for 3 hours in an air atmosphere. After heat treatment, the product is crushed and sieved to obtain a hexahedral nickel oxide precursor.
[0021] Furthermore, the preparation of the ring-shaped nickel oxide includes the following steps:
[0022] (1) Weigh according to proportion and NaOH, and Dissolve them together in 40 mL of distilled water and stir until completely dissolved to form a homogeneous solution;
[0023] (2) Transfer the homogeneous solution obtained in step (1) into a hydrothermal reactor, seal the reactor and place it in a temperature control device, and perform a hydrothermal reaction at 180°C for 5 hours. After the reaction is completed, a dark green suspension is obtained.
[0024] (3) The dark green suspension obtained in step (2) was centrifuged and separated. The centrifugation speed was controlled at 7000 rpm and the centrifugation time was 10 minutes. The solid product was collected.
[0025] (4) The solid product obtained in step (3) is placed in a vacuum oven at 60°C and dried overnight to obtain hexahedral nickel oxide precursor powder;
[0026] (5) The precursor powder obtained in step (4) is placed in a tube furnace and heat-treated at 500°C for 3 hours in an air atmosphere. After heat treatment, the product is crushed and sieved to obtain a hexahedral nickel oxide precursor.
[0027] Furthermore, when drying the solid product collected after centrifugation of the dark green suspension, the drying temperature is controlled at 60°C and the drying time is 5-12 hours.
[0028] Furthermore, when phosphating the precursor, a tube furnace is used as the reaction equipment. The precursor is placed in a quartz tube and then placed in the tube furnace. Phosphine gas is introduced to carry out the phosphating reaction. The process parameters for the phosphating reaction are: phosphine concentration of 1000 ppm, phosphating temperature of 380℃, phosphine gas flow rate of 100 mL / min, and phosphating reaction time of 400 min.
[0029] Furthermore, during the phosphating reaction, potassium permanganate solution and sodium hydroxide solution are used sequentially to treat the exhaust gas discharged from the tubular furnace.
[0030] Furthermore, the prepared Ni-containing x P y In electrocatalytic materials, the Ni x P y include .
[0031] The present invention has the following beneficial effects:
[0032] 1. This invention explores the differences in the adsorption performance of nickel oxide with different morphologies for phosphine. While achieving efficient removal of phosphine from tail gas, it also synthesizes an electrocatalyst material, thus achieving the dual goals of environmental protection and resource utilization. It has broad application prospects in the field of electrocatalytic water splitting for hydrogen production.
[0033] 2. The product prepared by this invention contains... The electrocatalytic material exhibits excellent electrocatalytic water splitting and hydrogen production performance in a 1 mol / L KOH electrolyte solution. Furthermore, the preparation method of this invention is simple, uses inexpensive and readily available raw materials, and achieves efficient removal of phosphine while preparing a high-performance electrocatalytic material, thus possessing the dual value of environmental protection and resource utilization. Attached Figure Description
[0034] Figure 1 These are SEM images of nickel oxides with different morphologies in the embodiments of the present invention;
[0035] Figure 2 This is a comparison diagram of the performance of nickel oxide phosphating materials with different morphologies prepared in the embodiments of the present invention;
[0036] Figure 3 This is a comparison diagram of the electrocatalytic performance of deactivated catalysts after phosphating nickel oxide with different morphologies in the embodiments of the present invention. Detailed Implementation
[0037] To enable those skilled in the art to better understand the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present application, and not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative effort should fall within the scope of protection of the present application.
[0038] Reference Figures 1-3 The specific embodiments of the present invention are as follows:
[0039] Example 1
[0040] Preparation and Phosphating of Octahedral Nickel Oxide
[0041] This embodiment discloses the preparation and phosphating process of octahedral nickel oxide (exposed (111) crystal planes), specifically including the following steps:
[0042] Solution preparation: Weigh out nickel nitrate crystals according to the specified proportion ( ), accurately measure 0.02 mol of Add it to 40 mL of anhydrous ethanol and stir with a magnetic stirrer until the solid is completely dissolved, forming a homogeneous and transparent solution.
[0043] Hydrothermal reaction: The homogeneous solution was transferred to a polytetrafluoroethylene-lined hydrothermal reactor. After sealing the reactor, it was placed in a programmable temperature-controlled oven at 110°C for 8 hours. After the reaction was completed, the oven power was turned off, and the reactor was allowed to cool naturally to room temperature. At this point, a dark green suspension was obtained in the reactor.
[0044] Centrifugation and drying: The dark green suspension was transferred to centrifuge tubes and centrifuged using a high-speed centrifuge. After centrifugation, the supernatant was discarded, and the solid product at the bottom of the tube was collected. The solid product was placed in a vacuum oven and dried at 60°C for 8 hours to obtain octahedral nickel oxide precursor powder.
[0045] Heat treatment: Octahedral nickel oxide precursor powder was placed in an alumina boat, which was then placed in a tube furnace. The temperature was raised to 400°C at a rate of 5°C / min in air and held for 2 hours. After the heat treatment, the tube furnace was allowed to cool naturally to room temperature. The product was then removed, crushed, and sieved to obtain the octahedral nickel oxide precursor.
[0046] Phosphating treatment: Weigh 0.05g of the above octahedral nickel oxide precursor and place it in a quartz tube. Place the quartz tube in the isothermal zone of a tube furnace. After sealing the tube furnace, first purge the air inside the tube with argon gas for 30 minutes (argon gas flow rate 100mL / min). Then purge with phosphine gas at a concentration of 1000ppm, controlling the phosphine flow rate at 100mL / min, and raise the temperature to 380℃ at a heating rate of 5℃ / min. Maintain this temperature for phosphating reaction for 400 minutes. After the reaction is complete, stop the phosphine gas flow, and continue to purge with argon gas until the tube furnace cools to room temperature, obtaining a product containing... Electrocatalytic materials.
[0047] Tail gas treatment: During the phosphating reaction, the tail gas discharged from the tubular furnace is sequentially passed into potassium permanganate solution and sodium hydroxide solution to complete the oxidation of residual phosphine and neutralization of acidic substances in the tail gas, thus avoiding environmental pollution from the tail gas.
[0048] Example 2
[0049] Preparation and Phosphating of Hexahedral Nickel Oxide
[0050] This embodiment discloses the preparation and phosphating process of hexahedral nickel oxide (exposed (110) crystal planes), specifically including the following steps:
[0051] Solution preparation: Weigh 0.04 mol of the solution according to the specified proportion. Add 0.01 mol NaOH together to 40 mL of distilled water and stir with a magnetic stirrer until the solid is completely dissolved to form a homogeneous mixed solution.
[0052] Hydrothermal reaction: The mixed solution was transferred to a polytetrafluoroethylene-lined hydrothermal reactor, sealed, and placed in a programmable temperature-controlled oven at 180°C for 5 hours. After the reaction, the solution was allowed to cool naturally to room temperature, yielding a dark green suspension.
[0053] Centrifugation: Transfer the dark green suspension to a centrifuge tube, centrifuge at 7000 rpm for 10 minutes, discard the supernatant, and collect the solid product.
[0054] Drying treatment: The solid product was placed in a vacuum oven at 60°C and dried overnight (drying time was about 12 hours) to obtain hexahedral nickel oxide precursor powder.
[0055] Heat treatment: The hexahedral nickel oxide precursor powder was placed in an alumina boat and then placed in a tube furnace. The temperature was raised to 500°C at a rate of 5°C / min under air atmosphere and held for 3 hours. After cooling, the product was crushed and sieved to obtain the hexahedral nickel oxide precursor.
[0056] Phosphating treatment: Weigh 0.05g of the above hexahedral nickel oxide precursor and place it in a quartz tube. Place the quartz tube in the isothermal zone of a tube furnace. After sealing the tube furnace, first purge the air inside the tube with argon gas for 30 minutes (argon gas flow rate 100mL / min). Then purge with phosphine gas at a concentration of 1000ppm, controlling the phosphine flow rate at 100mL / min, and raise the temperature to 380℃ at a heating rate of 5℃ / min. Maintain this temperature for phosphating reaction for 400 minutes. After the reaction is complete, stop the phosphine gas flow, and continue to purge with argon gas until the tube furnace cools to room temperature, obtaining a product containing... Electrocatalytic materials.
[0057] Tail gas treatment: During the phosphating reaction, the tail gas discharged from the tubular furnace is sequentially passed into potassium permanganate solution and sodium hydroxide solution to complete the oxidation of residual phosphine and neutralization of acidic substances in the tail gas, thus avoiding environmental pollution from the tail gas.
[0058] Example 3
[0059] Preparation and phosphating of cyclic nickel oxide
[0060] This embodiment discloses the preparation and phosphating process of annular nickel oxide, specifically including the following steps:
[0061] Solution preparation: Weigh 0.04 mol of the solution according to the specified proportion. Add 0.03 mol NaOH together to 40 mL of distilled water and stir until completely dissolved to form a homogeneous mixed solution.
[0062] Hydrothermal reaction: The mixed solution was transferred to a polytetrafluoroethylene-lined hydrothermal reactor, sealed, and placed in a programmable temperature-controlled oven. The hydrothermal reaction was carried out at 180°C for 5 hours. After natural cooling, a dark green suspension was obtained.
[0063] Centrifugation: Centrifuge the dark green suspension at 7000 rpm for 10 minutes, discard the supernatant, and collect the solid product.
[0064] Drying treatment: The solid product was placed in a vacuum oven at 60°C and dried overnight to obtain cyclic nickel oxide precursor powder.
[0065] Heat treatment: The annular nickel oxide precursor powder was placed in an alumina boat and placed in a tube furnace. It was heat-treated at 500°C for 3 hours in an air atmosphere. After cooling, it was crushed and sieved to obtain the annular nickel oxide precursor.
[0066] Phosphating treatment: Weigh 0.05g of the above-mentioned annular nickel oxide precursor and place it in a quartz tube. Place the quartz tube in the isothermal zone of a tube furnace. After sealing the tube furnace, first purge the air inside the tube with argon gas for 30 minutes (argon gas flow rate of 100mL / min). Then purge with phosphine gas at a concentration of 1000ppm, controlling the phosphine flow rate at 100mL / min, and raise the temperature to 380℃ at a heating rate of 5℃ / min. Maintain this temperature for phosphating reaction for 400 minutes. After the reaction is complete, stop the phosphine gas flow and continue to purge with argon gas until the tube furnace cools to room temperature, obtaining a product containing... Electrocatalytic materials.
[0067] Tail gas treatment: During the phosphating reaction, the tail gas discharged from the tubular furnace is sequentially passed into potassium permanganate solution and sodium hydroxide solution to complete the oxidation of residual phosphine and neutralization of acidic substances in the tail gas, thus avoiding environmental pollution from the tail gas.
[0068] The above-described embodiments yielded a product containing... The electrocatalytic material exhibits excellent electrocatalytic water splitting and hydrogen production performance in a 1 mol / L KOH electrolyte solution. Furthermore, the preparation method of this invention is simple, uses inexpensive and readily available raw materials, and achieves efficient removal of phosphine while preparing a high-performance electrocatalytic material, thus possessing the dual value of environmental protection and resource utilization.
[0069] As can be seen from the above embodiments, the present invention provides a method containing... Electrocatalytic materials have a relatively short preparation time, use inexpensive and readily available raw materials, are not limited by time or location, and do not produce side reactions; they have great application prospects in fields such as photoelectrocatalytic water splitting for hydrogen production and photocatalytic degradation of organic pollutants.
[0070] This invention explores the differences in the adsorption performance of nickel oxide with different morphologies for phosphine. While achieving efficient removal of phosphine from exhaust gas, it also synthesizes an electrocatalyst material, thus achieving the dual goals of environmental protection and resource utilization. This material has broad application prospects in the field of electrocatalytic water splitting for hydrogen production.
[0071] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented in orders other than those illustrated or described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.
[0072] Optionally, specific examples in this embodiment can refer to the examples described in the above embodiments, and will not be repeated here.
[0073] The sequence numbers of the embodiments in this application are for descriptive purposes only and do not represent the superiority or inferiority of the embodiments.
[0074] In the above embodiments of this application, the descriptions of each embodiment have different focuses. For parts not described in detail in a certain embodiment, please refer to the relevant descriptions of other embodiments.
[0075] The above description is only a preferred embodiment of this application. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of this application, and these improvements and modifications should also be considered within the scope of protection of this application.
Claims
1. A method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes, characterized in that, Using a nickel source as raw material, morphology-controllable nickel oxide particles with specific exposed crystal faces are synthesized via a solvothermal or hydrothermal method. The nickel oxide particles are then heat-treated to obtain a precursor, which is subsequently subjected to phosphating in a phosphine atmosphere to finally prepare a Ni-containing... x P y Electrocatalytic materials; wherein the specific crystal planes include (111) crystal planes and (110) crystal planes.
2. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 1, characterized in that, The nickel source is nickel nitrate, specifically... The morphology-controllable nickel oxide particles include octahedral nickel oxide, hexahedral nickel oxide and ring-shaped nickel oxide, with the octahedral nickel oxide exposing the (111) crystal plane and the hexahedral nickel oxide exposing the (110) crystal plane.
3. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 2, characterized in that, The preparation of the octahedral nickel oxide includes the following steps: (1) Weigh according to proportion ,Will It dissolves completely in 40 mL of anhydrous ethanol to form a homogeneous solution; (2) Transfer the homogeneous solution obtained in step (1) into a hydrothermal reactor, seal the reactor and place it in a temperature control device, and perform a hydrothermal reaction at 110°C for 8 hours. After the reaction is completed, a dark green suspension is obtained. (3) The dark green suspension obtained in step (2) is centrifuged to separate the solid product. The solid product is then placed in a vacuum oven to dry, and octahedral nickel oxide precursor powder is obtained. (4) The precursor powder obtained in step (3) is placed in a tube furnace and heat-treated at 400°C for 2 hours in an air atmosphere. After heat treatment, the product is crushed and sieved to obtain octahedral nickel oxide precursor.
4. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 2, characterized in that, The preparation of the hexahedral nickel oxide includes the following steps: (1) Weigh according to proportion ,Will and Dissolve them together in 40 mL of distilled water and stir until completely dissolved to form a homogeneous solution; (2) Transfer the homogeneous solution obtained in step (1) into a hydrothermal reactor, seal the reactor and place it in a temperature control device, and perform a hydrothermal reaction at 180°C for 5 hours. After the reaction is completed, a dark green suspension is obtained. (3) The dark green suspension obtained in step (2) was centrifuged and separated. The centrifugation speed was controlled at 7000 rpm and the centrifugation time was 10 minutes. The solid product was collected. (4) The solid product obtained in step (3) is placed in a vacuum oven at 60°C and dried overnight to obtain hexahedral nickel oxide precursor powder; (5) The precursor powder obtained in step (4) is placed in a tube furnace and heat-treated at 500°C for 3 hours in an air atmosphere. After heat treatment, the product is crushed and sieved to obtain a hexahedral nickel oxide precursor.
5. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 2, characterized in that, The preparation of the ring-shaped nickel oxide includes the following steps: (1) Weigh according to proportion and ,Will and Dissolve them together in 40 mL of distilled water and stir until completely dissolved to form a homogeneous solution; (2) Transfer the homogeneous solution obtained in step (1) into a hydrothermal reactor, seal the reactor and place it in a temperature control device, and perform a hydrothermal reaction at 180°C for 5 hours. After the reaction is completed, a dark green suspension is obtained. (3) The dark green suspension obtained in step (2) was centrifuged and separated. The centrifugation speed was controlled at 7000 rpm and the centrifugation time was 10 minutes. The solid product was collected. (4) The solid product obtained in step (3) is placed in a vacuum oven at 60°C and dried overnight to obtain hexahedral nickel oxide precursor powder; (5) The precursor powder obtained in step (4) is placed in a tube furnace and heat-treated at 500°C for 3 hours in an air atmosphere. After heat treatment, the product is crushed and sieved to obtain a hexahedral nickel oxide precursor.
6. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 3, 4, or 5, characterized in that, When drying the solid product collected after centrifugation of the dark green suspension, the drying temperature is controlled at 60℃ and the drying time is 5-12h.
7. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 1, characterized in that, When phosphating the precursor, a tube furnace is used as the reaction equipment. The precursor is placed in a quartz tube and then placed in the tube furnace. Phosphine gas is introduced to carry out the phosphating reaction. The process parameters of the phosphating reaction are: phosphine concentration of 1000 ppm, phosphating temperature of 380℃, phosphine gas flow rate of 100 mL / min, and phosphating reaction time of 400 min.
8. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 7, characterized in that, During the phosphating reaction, potassium permanganate solution and sodium hydroxide solution are used to treat the exhaust gas discharged from the tubular furnace in sequence.
9. The method for preparing an electrocatalyst by controlling the adsorption of phosphine via nickel oxide crystal planes according to claim 1, characterized in that, Ni-containing x P y In electrocatalytic materials, the Ni x P y include .