CN114892235A - Method for screening micro-arc oxidation process electrolyte by using electrochemical means - Google Patents
Method for screening micro-arc oxidation process electrolyte by using electrochemical means Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/30—Anodisation of magnesium or alloys based thereon
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- 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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention provides a method for screening micro-arc oxidation process electrolyte through an electrochemical polarization curve, which comprises the steps of taking the micro-arc oxidation process electrolyte as an electrolyte solution, adopting a three-electrode system and taking metal to be plated as a working electrode to carry out an anodic polarization test. And analyzing the anode region of the voltage-current density curve obtained by testing, and exploring the passivation behavior of the metal to be plated in the electrolyte. And then judging whether the electrolyte can rapidly form a passive film on the alloy surface under the condition of external current so as to support the subsequent micro-arc oxidation process. The method provided by the invention does not need complicated working procedures, does not need to prepare a large amount of electrolyte for experiments, only needs to prepare enough solution for electrochemical experiments, is connected with an electrochemical workstation for testing, and can be used as a means for rapidly screening the electrolyte for the micro-arc oxidation process. The experimental result is real, stable and reliable, and the time cost and the economic cost can be saved.
Description
Technical Field
The invention relates to the technical field of metal surface protection treatment, in particular to a method for screening micro-arc oxidation process electrolyte by using an electrochemical means.
Background
The light metal and the alloy thereof have the characteristics of low density, high strength-to-weight ratio and the like, have good electromagnetic shielding, higher damping capacity and high machinability, and have wide application in the fields of automobiles, aerospace, communication, biodegradable medical implant materials and the like. However, the high reactivity of light metals impairs their corrosion and wear resistance, especially in corrosive media. Therefore, the surface performance of the material can be improved and the service life of the material can be prolonged by carrying out proper surface treatment on the material. Several surface treatment techniques are currently used to protect light metals and their alloys, such as chemical conversion plating, electrodeposition, anodization, vapor deposition, organic coatings, and sol-gel techniques.
The micro-arc oxidation technology is a surface treatment technology which is started in recent years, is derived from the traditional anodic oxidation technology, is an economic and environment-friendly technology, and has wide application. In the micro-arc oxidation process, a ceramic film layer is formed on the surface of valve metal such as Mg, Al, Ti and the like in situ through the combined action of plasma chemistry, electrochemistry and thermochemistry. The oxide film prepared by the technology has compact structure, strong binding force and excellent comprehensive mechanical property.
The formation mechanism of the micro-arc oxidation film layer is always a hot spot of attention, but the formation mechanism is a very complicated process and comprises a plurality of electrochemical, chemical and plasma chemical reactions. According to the current research, the micro-arc oxidation process can be divided into: anode oxidation, spark discharge, micro-arc discharge and arc discharge. In the initial stage of micro-arc oxidation, anodic oxidation occurs on the surface of the metal alloy as an anode, a large number of bubbles are generated on the surface, and the metallic luster disappears. At this stage, oxygen molecules and hydroxyl anions in the solution are adsorbed, and a thin passivation film is formed on the surface of the metal. With the increase of voltage, the passivation film can be repeatedly broken down, and finally a micro-arc oxidation ceramic layer with a compact structure grows in situ on the metal surface. Therefore, if a passivation film with a compact structure can be quickly formed on the surface of the alloy, the micro-arc oxidation process can enter a spark discharge stage in advance, and the growth of the film layer is facilitated.
The breakdown voltage of the passivation film greatly depends on the concentration and conductivity of the electrolyte, and the components of the electrolyte also influence the performance of the micro-arc oxidation process and the prepared film. Therefore, research on the electrolyte of the micro-arc oxidation process is always a hotspot in the field. However, finding a suitable micro-arc oxidation process electrolyte requires a great deal of time and energy consumption of scientific research personnel. Usually, in order to achieve the purpose of screening, a large amount of electrolytes with different concentrations and components need to be prepared to prepare a micro-arc oxidation film layer on the metal alloy, and then a proper electrolyte is screened out through comparison, so that a lot of unnecessary waste is caused in the process. Therefore, there is a need for improved means for screening electrolytes for micro-arc oxidation processes.
In view of this, the invention is particularly proposed.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for screening the electrolyte of the micro-arc oxidation process by an electrochemical means. Since corrosion generally occurs through electrochemical reactions, electrochemical techniques are used to study the corrosion process, and polarization is one of the most common of the numerous electrochemical techniques that can be used to determine the rate of metal corrosion. The polarization curve can be divided into a cathodic polarization curve and an anodic polarization curve, which respectively represent the cathodic reduction reaction and the oxidation reaction of the metal electrode (working electrode) in the whole experimental process. When anodic polarization of metal proceeds to a relatively high potential, a solid-phase surface film, that is, an anodic passivation film, is formed on the metal surface.
The invention pours the electrolyte for micro-arc oxidation process into the electrochemical electrolytic cell, the metal sample is used as the working electrode to contact with the electrolyte, and the metal sample is anode polarized to a higher potential. And data acquisition is carried out in the process, and whether a steady-state passivation area exists in the electrolyte or not is judged by drawing the data into an anode polarization curve. In the region, the current density does not change with the change of the potential, and a passivation film is formed on the metal surface. If a passivation region which is obvious and has a large potential range appears, the metal can be passivated in the electrolyte, and then the micro-arc oxidation film layer can be prepared. By the method, the electrolyte which cannot be prepared on the metal to be plated with the micro-arc oxidation film layer can be more quickly and accurately removed, and the electrolyte which is more suitable for preparing the micro-arc oxidation film layer on the metal to be plated is screened out.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention relates to a method for screening micro-arc oxidation process electrolyte by an electrochemical means, which comprises the following steps:
(1) preparing micro-arc oxidation process electrolyte to be screened, and pretreating metal to be plated;
preferably, the micro-arc oxidation process electrolyte mainly refers to an alkaline micro-arc oxidation electrolyte, and is selected from any one or composite electrolyte of basic electrolyte systems such as a silicate system, a phosphate system, an aluminate system and the like. The electrolyte contains main salt and hydroxide, wherein the main salt is selected from at least one of silicate, phosphate and aluminate, and the hydroxide is selected from at least one of sodium hydroxide and potassium hydroxide.
Further, the silicate system is an electrolyte system mainly containing silicate, and mainly contains sodium silicate and hydroxide (sodium hydroxide, potassium hydroxide, etc.). The phosphate system is an electrolyte system mainly composed of phosphate, and mainly contains sodium dihydrogen phosphate, trisodium phosphate, sodium pyrophosphate, and hydroxide (sodium hydroxide, potassium hydroxide, etc.). The aluminate system is an electrolyte system mainly comprising aluminate and mainly comprises sodium aluminate and hydroxide (sodium hydroxide, potassium hydroxide and the like). The composite electrolyte system refers to an electrolyte system containing a plurality of main salts, such as silicate-aluminate, silicate-phosphate, aluminate-molybdate and the like. In general, the concentration of the main salt such as silicate, phosphate, aluminate, etc. in the electrolyte is 5 to 100g/L, the concentration of the hydroxide such as sodium hydroxide, potassium hydroxide, etc. in the electrolyte is 1 to 50g/L, and the pH of the electrolyte system is controlled to 7 or more.
In addition, additives can be added into different electrolyte systems to improve the stability and conductivity of the electrolyte, improve the quality of the film and adjust the structure of the film. The micro-arc oxidation additive is mostly solid particles, soluble salts and organic matters. Wherein the particulate additive comprises: TiO 2 2 Particles, ZrO 2 Particles of Al 2 O 3 Particles of metal oxides, e.g. of TiO 2 Sol particles such as sol and alumina sol; the inorganic additives include: borax, metal inorganic salts (sodium fluoride, potassium fluoride, etc.), acetates, zirconates, phosphates, etc.; the organic additives include: ethanol, glycerol, phytic acid, and the like. The addition amount of the additive is adjusted along with the change of the concentration of the main salt, and the additive and the main salt are matched to improve some properties of the micro-arc oxidation film layer, such as thickness, hardness, roughness, wear resistance, corrosion resistance and the like. In general, the concentration of the additive is in the range of 0 to 30 g/L.
Preferably, the metal to be plated is a light metal or an alloy thereof, and is selected from one of pure aluminum, pure magnesium, pure titanium, aluminum alloy, magnesium alloy and titanium alloy. Wherein the aluminum alloy includes 1-series, 2-series, 3-series, 4-series, 5-series, 6-series, and 7-series aluminum alloys. The magnesium alloy includes AZ, AS, AE, LA series magnesium alloy, etc. The titanium alloy includes TA, TC, TB, ZTC titanium alloy, etc.
Preferably, the pretreatment comprises sequentially grinding, polishing, cleaning and drying the metal to be plated.
(2) Electrochemical anodic polarization test: pouring the micro-arc oxidation process electrolyte to be screened prepared in the step (1) into an electrochemical electrolytic cell, taking the pretreated metal to be plated as a working electrode, and configuring a reference electrode and a counter electrode to perform an electrochemical anodic polarization test;
preferably, the reference electrode is an Ag/AgCl electrode, the counter electrode is a platinum electrode, and the working electrode, the reference electrode and the counter electrode are all in contact with the electrolyte in a certain area.
Preferably, the electrochemical anodic polarization test comprises: and selecting a dynamic potential scanning mode in electrochemical software, wherein the potential is set to be scanned from negative to positive by taking any value within a range of 0.05-0.5V below the open-circuit potential as a starting point, and the scanning rate is 1-10 mV/s.
(3) Drawing a voltage-current density curve according to the measured electrochemical data, analyzing the passivation behavior of the metal to be plated in the electrolyte according to the curve,
if a stable state passivation area exists in the curve, the electrolyte can be used as a micro-arc oxidation electrolyte of the metal to be plated;
if the stable state passivation area does not exist in the curve, the electrolyte cannot be used as the micro-arc oxidation electrolyte of the metal to be plated;
preferably, the steady state passivation region is defined as: in the region, the current density does not change along with the change of the potential, and a passivation film is formed on the surface of the metal to be plated. Whether the metal can be passivated in the electrolyte can be judged, the electrolyte is rapidly screened, and support is provided for the subsequent micro-arc oxidation experiment.
The invention has the beneficial effects that:
the invention provides a method for screening micro-arc oxidation process electrolyte through an electrochemical polarization curve, which comprises the steps of taking the micro-arc oxidation process electrolyte as an electrolyte solution, adopting a three-electrode system and taking metal to be plated as a working electrode to carry out an anodic polarization test. And analyzing the anode region of the voltage-current density curve obtained by testing, and exploring the passivation behavior of the metal to be plated in the electrolyte. And then judging whether the electrolyte can rapidly form a passive film on the alloy surface under the condition of external current so as to support the subsequent micro-arc oxidation process.
The method provided by the invention does not need complicated working procedures, does not need to prepare a large amount of electrolyte for experiments, only needs to prepare enough solution for electrochemical experiments, is connected with an electrochemical workstation for testing, and can be used as a means for rapidly screening the electrolyte for the micro-arc oxidation process. The experimental result is real, stable and reliable, and the time cost and the economic cost can be saved.
Drawings
FIG. 1 is a graph of potential versus current density obtained by electrochemical anodic polarization testing of a magnesium-lithium alloy in an electrolyte according to example 1 of the present invention;
FIG. 2 is a voltage-time curve obtained by performing a micro-arc oxidation experiment on a magnesium-lithium alloy in the electrolyte of embodiment 1 of the invention.
FIG. 3 is a graph of potential versus current density obtained from electrochemical anodic polarization testing of aluminum alloys in the electrolyte of example 2 of the present invention;
FIG. 4 is a voltage-time curve obtained by performing a micro-arc oxidation experiment on an aluminum alloy in the electrolyte of example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a method for screening micro-arc oxidation process electrolyte by using an electrochemical means, which comprises the following steps:
(1) preparation of micro-arc oxidation process electrolyte
Three electrolytes were prepared, respectively: deionized water and electrolyte 1 (electrolyte component: 10 g/LNa) 2 SiO 3 、5g/L KOH、1.5g/L(NaPO 3 ) 6 1g/L NaF), electrolyte 2 (electrolyte component: 20g/L Na 2 SiO 3 、40g/L NaOH、25g/L Na 2 B 4 O 7 、15g/L Na 3 C 6 H 5 O 7 ·2H 2 O). Both electrolytes 1 and 2 are silicate electrolytes.
(2) Pretreatment of metal surfaces
Taking a LA91 magnesium-lithium alloy sheet with the size of 40mm long, 40mm wide and 5mm thick, sequentially grinding the sheet by using 200#, 400#, 800#, 1200# and 2000# silicon carbide abrasive paper, polishing the sheet to a mirror surface by using diamond polishing paste, and then ultrasonically cleaning and drying the sheet by using deionized water and acetone;
(3) electrochemical anodic polarization test
Pouring the three electrolytes prepared in the step (1) into an electrochemical electrolytic cell container respectively, taking the metal pretreated in the step (2) as a working electrode, and mixing the working electrode with the electrolytes by 1cm 2 Area contact, the reference electrode is an Ag/AgCl electrode, the counter electrode is a platinum electrode, and electrochemical polarization test is carried out. The electrochemical workstation was purchased from Wuhan Const instruments Inc. under model number CS350/CS 16X. The potential was set in the electrochemical workstation software to sweep from negative to positive over a wide range from 0.1V below the open circuit potential at a sweep rate of 10 mV/s.
FIG. 1 is a graph of potential versus current density (V-log I) plotted against measured electrochemical data. It can be seen from the figure that the curves corresponding to the electrolyte 1 and the electrolyte 2 can find a steady-state passivation region, and in this region, the current density hardly changes with the change of the potential, i.e. the ab and cd sections in fig. 1, which shows that when current is applied in the two systems, a passivation film can be rapidly formed on the surface of the magnesium-lithium alloy. The curve obtained by testing in deionized water has no obvious steady-state passivation region, i.e. a stable and continuous passivation film cannot be formed in deionized water. It is concluded that both electrolyte 1 and electrolyte 2 can be used as micro-arc oxidation electrolyte, while deionized water cannot be used as micro-arc oxidation electrolyte.
In order to verify the truth and effectiveness of the experimental results, the micro-arc oxidation film layer is directly prepared in the three electrolyte systems. Wherein, the magnesium-lithium alloy can be discharged in the electrolyte 1 and the electrolyte 2 to successfully prepare the micro-arc oxidation film layer, and the corresponding voltage-time curve is shown in figure 2. And the micro-arc oxidation film layer can not be prepared by arc striking and discharging in deionized water. The results are in full agreement with the results of the electrochemical experiments.
Example 2
The embodiment provides a method for screening micro-arc oxidation process electrolyte by using an electrochemical means, which comprises the following steps:
(1) preparation of micro-arc oxidation process electrolyte
Three electrolytes were prepared, respectively: deionized water, electrolyte 1 (electrolyte component: 10 g/LNa) 2 SiO 3 、5g/L KOH、1.5g/L(NaPO 3 ) 6 1g/L NaF), electrolyte 2 (electrolyte composition: 40g/L NaOH, 20g/L Na 2 SiO 3 、25g/L Na 2 B 4 O 7 、15g/L Na 3 C 6 H 5 O 7 ·2H 2 O). Both electrolytes 1 and 2 are silicate electrolytes.
(2) Pretreatment of metal surfaces
Taking a 2024 aluminum alloy sheet with the size of 40mm long, 40mm wide and 5mm thick, sequentially grinding by using 200#, 400#, 800#, 1200# and 2000# silicon carbide abrasive papers, polishing to a mirror surface by using diamond polishing paste, and then ultrasonically cleaning and drying by using deionized water and acetone;
(3) electrochemical anodic polarization test
Pouring the three electrolytes prepared in the step (1) into an electrochemical electrolytic cell container respectively, taking the metal pretreated in the step (2) as a working electrode, and mixing with the electrolytes by 1cm 2 Area contact, the reference electrode is an Ag/AgCl electrode, the counter electrode is a platinum electrode, and electrochemical polarization test is carried out. The potential was set in the electrochemical software to sweep from negative to positive over a wide range from 0.1V below the open circuit potential at a sweep rate of 10 mV/s.
Fig. 3 is a potential-current density curve plotted according to measured electrochemical data, and it can be seen from the graph that the steady-state passivation region can be found by the corresponding curves of the electrolyte 1 and the electrolyte 2. In this region, the current density hardly changes with the potential change, i.e. ef, gh in fig. 3, which shows that the aluminum alloy surface can rapidly form a passivation film when current is applied in the two electrolyte systems. The curve obtained by testing in deionized water has no obvious steady-state passivation region, i.e. a stable and continuous passivation film cannot be formed in deionized water. It is concluded that both electrolyte 1 and electrolyte 2 can be used as micro-arc oxidation electrolyte, while deionized water cannot be used as micro-arc oxidation electrolyte.
In order to verify that the experimental results are real and effective, the micro-arc oxidation film layer is directly prepared in three systems, wherein aluminum alloy can be subjected to arc striking discharge in the electrolysis 1 and the electrolyte 2 to successfully prepare the micro-arc oxidation film layer, the corresponding voltage-time curve is shown in fig. 4, and the micro-arc oxidation film layer cannot be prepared when the experiment is carried out in deionized water, namely the micro-arc oxidation film layer cannot be subjected to arc striking discharge. The results are in full agreement with the results of the electrochemical experiments. The electrochemical test method can be used as a means for screening the micro-arc oxidation electrolyte.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. A method for screening micro-arc oxidation process electrolyte by an electrochemical means is characterized by comprising the following steps:
(1) preparing micro-arc oxidation process electrolyte to be screened, and pretreating metal to be plated;
(2) electrochemical anodic polarization test: pouring the micro-arc oxidation process electrolyte to be screened prepared in the step (1) into an electrochemical electrolytic cell, taking the pretreated metal to be plated as a working electrode, and configuring a reference electrode and a counter electrode to perform an electrochemical anodic polarization test;
(3) drawing a voltage-current density curve according to the measured electrochemical data, analyzing the passivation behavior of the metal to be plated in the electrolyte according to the curve,
if a stable state passivation area exists in the curve, the electrolyte is used as the micro-arc oxidation electrolyte of the metal to be plated;
if no steady state passivation region exists in the curve, the electrolyte cannot be used as the micro-arc oxidation electrolyte of the metal to be plated.
2. The method according to claim 1, wherein in step (1), the micro-arc oxidation process electrolyte is an alkaline micro-arc oxidation electrolyte, and is selected from any one of silicate electrolyte, phosphate electrolyte and aluminate electrolyte or a composite electrolyte.
3. The method according to claim 2, wherein in the step (1), the electrolyte contains a main salt and a hydroxide, wherein the main salt is selected from at least one of silicate, phosphate and aluminate, and the hydroxide is selected from at least one of sodium hydroxide and potassium hydroxide.
4. The method according to claim 3, wherein in the step (1), the concentration of the main salt in the electrolyte is in the range of 5 to 100g/L, and the concentration of the hydroxide in the electrolyte is in the range of 1 to 50 g/L.
5. The method according to claim 1, wherein in the step (1), the metal to be plated is a light metal or an alloy thereof, and is selected from one of pure aluminum, pure magnesium, pure titanium, aluminum alloy, magnesium alloy and titanium alloy.
6. The method according to claim 1, wherein in the step (1), the pretreatment comprises sequentially performing grinding, polishing, cleaning and drying on the metal to be plated.
7. The method of claim 1, wherein in step (2), the reference electrode is an Ag/AgCl electrode and the counter electrode is a platinum electrode.
8. The method of claim 1, wherein in step (2), the electrochemical anodic polarization test comprises: and selecting a dynamic potential scanning mode in electrochemical software, wherein the potential is set to be scanned from negative to positive by taking any value within a range of 0.05-0.5V below the open-circuit potential as a starting point, and the scanning rate is 1-10 mV/s.
9. The method of claim 1, wherein in step (3), the steady state passivation region is defined as: in the region, the current density does not change along with the change of the potential, and a passivation film is formed on the surface of the metal to be plated.
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| US20110221445A1 (en) * | 2008-11-26 | 2011-09-15 | Constanze Donner | Method for control of stabilizer additives in electroless metal and metal alloy plating electrolytes |
| CN102409371A (en) * | 2011-11-29 | 2012-04-11 | 哈尔滨工业大学 | Method for detecting micro-arc oxidation arcing characteristics of alloy by using anodic polarization curve |
| CN109402699A (en) * | 2018-11-01 | 2019-03-01 | 中国科学院兰州化学物理研究所 | A kind of aluminum alloy surface acid resistance corrosion function ceramic membrane preparation process |
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