CN114420925A - Preparation method of n-type cuprous phosphide - Google Patents

Preparation method of n-type cuprous phosphide Download PDF

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Publication number
CN114420925A
CN114420925A CN202210057770.4A CN202210057770A CN114420925A CN 114420925 A CN114420925 A CN 114420925A CN 202210057770 A CN202210057770 A CN 202210057770A CN 114420925 A CN114420925 A CN 114420925A
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cuprous phosphide
copper foil
phosphide
corundum
cuprous
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CN114420925B (en
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彭雪
吕燕飞
蔡庆锋
席俊华
傅力
陈飞
张睿
赵士超
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Hangzhou Dianzi University
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Hangzhou Dianzi University
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    • H—ELECTRICITY
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5805—Phosphides
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/08—Other phosphides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C01G9/03—Processes of production using dry methods, e.g. vapour phase processes
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
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    • C25B1/04—Hydrogen or oxygen by electrolysis of water
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    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • H—ELECTRICITY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • 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
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    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a preparation method of n-type cuprous phosphide, which comprises the following steps: s1, preparing a copper foil with cuprous phosphide growing on the surface; s2, taking the copper foil with the cuprous phosphide growing on the surface as a substrate, and depositing a zinc oxide film on the surface; s3, heating the product prepared in the step S2 in inert gas, wherein the heat treatment temperature is 650-750 ℃, and the heat preservation time is 60-300 min. By adopting the technical scheme, the cuprous phosphide continuous film grows on the surface of the copper foil, the zinc oxide film is deposited on the surface of the cuprous phosphide by magnetron sputtering, zinc oxide and the cuprous phosphide interact at high temperature, and zinc and oxygen elements diffuse into cuprous phosphide lattices to form n-type doped cuprous phosphide.

Description

Preparation method of n-type cuprous phosphide
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a preparation method of n-type cuprous phosphide.
Background
The cuprous phosphide is a semiconductor material and has application in the fields of lithium ion battery electrode materials, photocatalytic decomposition of organic matters, electrocatalytic hydrogen production and the like. The semiconductor material can change the carrier concentration, the conductivity type and other properties through doping, for example, boron, sulfur, cobalt and oxygen doping can be found to improve the catalytic performance of the semiconductor material. However, only p-type cuprous phosphide exists in the market at present, and research and improvement on the p-type cuprous phosphide are realized. So far, no relevant report of n-type cuprous phosphide exists.
Disclosure of Invention
According to the defects of the prior art, the invention provides the preparation method of the n-type cuprous phosphide, the n-type cuprous phosphide is prepared by doping, and the preparation method has the advantages of low resistivity, high thermoelectric force and quick photoelectric reaction.
The technical scheme of the invention is as follows:
a preparation method of n-type cuprous phosphide comprises the following steps:
s1, preparing a copper foil with cuprous phosphide growing on the surface;
s2, taking the copper foil with the cuprous phosphide growing on the surface as a substrate, and depositing a zinc oxide film on the surface;
s3, heating the product prepared in the step S2 in inert gas, wherein the heat treatment temperature is 650-750 ℃, and the heat preservation time is 60-300 min.
Preferably, in step S2, the surface of the copper foil with the cuprous phosphide grown thereon is deposited with a zinc oxide film by magnetron sputtering.
Preferably, the vacuum degree of the equipment used in the magnetron sputtering method is 0.1-1.0Pa, the oxygen flow is 1-5sccm, the argon flow is 20-50sccm, the sputtering voltage is 300-450V, the current is 30-60mA, the sputtering time is 20-40min, and the target material is a metallic zinc target.
Preferably, the thickness of the zinc oxide film prepared by the magnetron sputtering method is 50-200 nm.
Preferably, the preparation method of step S1 is as follows:
s1-1, putting sodium hypophosphite into the corundum boat, and then covering the surface of the corundum boat with 1-5 square centimeters of copper foil with the thickness of 250-1000 microns;
s1-2, placing the corundum boat obtained in the step S1-1 into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
s1-3, heating the corundum tube in the step S1-2 to 280-300 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; the temperature is increased to 280-300 ℃ and then is kept for 30-60 min; and naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out the copper foil with cuprous phosphide growing on the surface of the product.
Preferably, the copper foil has a thickness of 600 μm.
The invention has the following characteristics and beneficial effects:
by adopting the technical scheme, the cuprous phosphide continuous film is deposited and grown on the surface of the copper foil, the zinc oxide film is deposited on the surface of the cuprous phosphide by using magnetron sputtering, zinc oxide and the cuprous phosphide interact at high temperature, and zinc and oxygen elements are diffused into cuprous phosphide lattices to form n-type doped cuprous phosphide.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is an X-ray diffractogram of n-type cuprous phosphide prepared by the example of the present invention;
FIG. 2 is a graph showing the variation of the temperature difference potential of cuprous phosphide prepared by the example of the present invention with the heating condition.
Detailed Description
Example 1
The embodiment provides a preparation method of n-type cuprous phosphide, which comprises the following steps:
s1, preparing a copper foil with cuprous phosphide growing on the surface;
s1-1, putting sodium hypophosphite into a corundum boat, and then covering a copper foil with the thickness of 250 microns, wherein the surface of the corundum boat is 1 square centimeter;
s1-2, placing the corundum boat obtained in the step S1-1 into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
s1-3, heating the corundum tube obtained in the step S1-2 to 280 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 30min after the temperature is raised to 280 ℃; then naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out the copper foil with cuprous phosphide growing on the surface of the product;
s2, taking the product obtained in the step S1 as a substrate, and depositing a zinc oxide film by a magnetron sputtering method; the vacuum degree of the magnetron sputtering equipment is 0.1Pa, the oxygen flow is 1sccm, the argon flow is 20sccm, the sputtering voltage is 300V, the current is 30mA, the sputtering time is 20min, and the target material is a metal zinc target; the thickness of the prepared zinc oxide film is 50 nm;
s3, heating the product of the step S2 in inert gas to form n-type semiconductor cuprous phosphide; the heat treatment temperature is 650 ℃, and the heat preservation time is 120 min.
According to the technical scheme, the cuprous phosphide continuous film is deposited and grown on the surface of the copper foil, the zinc oxide film is deposited on the surface of the cuprous phosphide by magnetron sputtering, zinc oxide and the cuprous phosphide interact at high temperature, and zinc and oxygen elements diffuse into cuprous phosphide lattices to form n-type doped cuprous phosphide.
It should be noted that the copper foil substrate in this embodiment may also be a silicon substrate.
In this embodiment, the zinc oxide is deposited on the surface of the cuprous phosphide by a magnetron sputtering method, and the method can also be a physical method such as a sol-gel method, a chemical vapor deposition method, a laser pulse deposition method, and the like.
Example 2
The present embodiment is different from embodiment 1 in that it includes the following steps:
s1, preparing a copper foil with cuprous phosphide growing on the surface;
s1-1, putting sodium hypophosphite into a corundum boat, and then covering a copper foil with the thickness of 500 microns, wherein the surface of the corundum boat is 3 square centimeters;
s1-2, placing the corundum boat obtained in the step S1-1 into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
s1-3, heating the corundum tube obtained in the step S1-2 to 290 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature after the temperature is increased to 290 ℃, wherein the heat preservation time is 40 min; then naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out the copper foil with cuprous phosphide growing on the surface of the product;
s2, taking the product obtained in the step S1 as a substrate, and depositing a zinc oxide film by a magnetron sputtering method; the vacuum degree of the magnetron sputtering equipment is 0.6Pa, the oxygen flow is 3sccm, the argon flow is 40sccm, the sputtering voltage is 400V, the current is 40mA, the sputtering time is 30min, and the target material is a metal zinc target; the thickness of the prepared zinc oxide film is 120 nm;
s3, heating the product of the step S2 in inert gas to finally form n-type semiconductor cuprous phosphide; the heat treatment temperature is 700 ℃, and the heat preservation time is 180 min.
Example 3
The present embodiment is different from embodiment 1 in that it includes the following steps:
s1, preparing a copper foil with cuprous phosphide growing on the surface;
s1-1, putting sodium hypophosphite into a corundum boat, and then covering a copper foil with the thickness of 1000 microns, wherein the surface of the corundum boat is 5 square centimeters;
s1-2, placing the corundum boat obtained in the step S1-1 into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
s1-3, heating the corundum tube obtained in the step S1-2 to 300 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 60min after the temperature is raised to 300 ℃; then naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out the copper foil with cuprous phosphide growing on the surface of the product;
s2, taking the product obtained in the step S1 as a substrate, and depositing a zinc oxide film by a magnetron sputtering method; the vacuum degree of the magnetron sputtering equipment is 1.0Pa, the oxygen flow is 5sccm, the argon flow is 50sccm, the sputtering voltage is 450V, the current is 60mA, the sputtering time is 40min, and the target material is a metal zinc target; the thickness of the prepared zinc oxide film is 200 nm;
s3, heating the product of the step S2 in inert gas to form n-type semiconductor cuprous phosphide; the heat treatment temperature is 750 ℃, and the heat preservation time is 300 min.
With reference to the n-type cuprous phosphide prepared in examples 1 to 3, as shown in fig. 1, it is apparent that the X-ray diffraction peaks of the n-type cuprous phosphide prepared in examples 1 to 3, wherein 43, 74 and 90 ° are diffraction peaks of copper crystals, and diffraction peaks at other positions are from the n-type cuprous phosphide, so that the n-type cuprous phosphide prepared by the technical scheme provided by the present example has the advantages of simple preparation method, good repeatability, low cost, low resistivity, high thermoelectromotive force and fast photoelectric response.
In addition, as can be seen from fig. 2, the manufactured n-type cuprous phosphide thermoelectromotive force changes with heating time, and in the figure, the abscissa represents time and the ordinate represents a potential value. After the anode is heated, the potential is a positive value, which indicates that the doped cuprous phosphide is an n-type semiconductor, namely n-type cuprous phosphide.

Claims (6)

1. The preparation method of the n-type cuprous phosphide is characterized by comprising the following steps of:
s1, preparing a copper foil with cuprous phosphide growing on the surface;
s2, taking the copper foil with the cuprous phosphide growing on the surface as a substrate, and depositing a zinc oxide film on the surface;
s3, heating the product prepared in the step S2 in inert gas, wherein the heat treatment temperature is 650-750 ℃, and the heat preservation time is 60-300 min.
2. The method for preparing n-type cuprous phosphide, according to claim 1, wherein in said step S2, said surface of copper foil with cuprous phosphide grown thereon is subjected to magnetron sputtering to deposit zinc oxide film.
3. The preparation method of n-type cuprous phosphide as claimed in claim 2, wherein the vacuum degree of the equipment used in magnetron sputtering method is 0.1-1.0Pa, the oxygen flow is 1-5sccm, the argon flow is 20-50sccm, the sputtering voltage is 300-450V, the current is 30-60mA, the sputtering time is 20-40min, and the target material is metallic zinc target.
4. The preparation method of n-type cuprous phosphide according to claim 2, characterized in that the thickness of zinc oxide film prepared by magnetron sputtering method is 50-200 nm.
5. The preparation method of n-type cuprous phosphide according to claim 1, characterized by comprising the following steps of S1:
s1-1, putting sodium hypophosphite into the corundum boat, and then covering the surface of the corundum boat with 1-5 square centimeters of copper foil with the thickness of 250-1000 microns;
s1-2, placing the corundum boat obtained in the step S1-1 into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
s1-3, heating the corundum tube in the step S1-2 to 280-300 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature after the temperature is increased to 280-300 ℃, wherein the heat preservation time is 30-60 min; and naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out the copper foil with cuprous phosphide growing on the surface of the product.
6. The method for preparing n-type cuprous phosphide of claim 1, wherein the thickness of said copper foil is 600 μm.
CN202210057770.4A 2022-01-19 2022-01-19 Preparation method of n-type cuprous phosphide Active CN114420925B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104979556A (en) * 2015-05-15 2015-10-14 三峡大学 Nitrogen-doped Cu3P/C-Cu lithium-ion battery negative electrode material and preparation method thereof
CN111564610A (en) * 2020-04-03 2020-08-21 华南师范大学 Carbon-coated cuprous phosphide-copper composite particle modified by carbon nanotube and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104979556A (en) * 2015-05-15 2015-10-14 三峡大学 Nitrogen-doped Cu3P/C-Cu lithium-ion battery negative electrode material and preparation method thereof
CN111564610A (en) * 2020-04-03 2020-08-21 华南师范大学 Carbon-coated cuprous phosphide-copper composite particle modified by carbon nanotube and preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
SHIXIN HUA等: ""Highly efficient p-type Cu3P/n-type g-C3N4 photocatalyst through Z-scheme charge transfer route"", 《APPLIED CATALYSIS B: ENVIRONMENTAL》, vol. 240 *
魏杰顶;徐小丽;: "Cu_3P纳米阵列的低温合成及其影响因素", 广东化工, no. 01 *

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