CN100396823C - Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology - Google Patents
Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology Download PDFInfo
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- CN100396823C CN100396823C CNB2005100960878A CN200510096087A CN100396823C CN 100396823 C CN100396823 C CN 100396823C CN B2005100960878 A CNB2005100960878 A CN B2005100960878A CN 200510096087 A CN200510096087 A CN 200510096087A CN 100396823 C CN100396823 C CN 100396823C
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Abstract
The present invention relates to a method and a device thereof for preparing coatings or thin films by ultrasonic hydrothermal electric deposition. The device comprises a hydrothermal kettle and electrodes arranged in the hydrothermal kettle and connected with a power supply; the outer side of the hydrothermal kettle is also provided with an ultrasonic wave generating groove connected with an ultrasonic generator, and the ultrasonic wave generating groove is communicated with a thermostatic groove through a liquid outlet liquid returning pipe. The present invention has the technical scheme that the negative electrode and the positive electrode are arranged in the reactive hydrothermal kettle, and thus, the electric deposition is combined with hydrothermal deposition; the temperature of the hydrothermal kettle is controlled by the thermostatic groove, and compact coatings or thin films are directly synthesized in the supercritical condition; later-stage thermal treatment is avoided by controlling the deposition thickness through electric deposition. The present invention has the advantages of simple preparation process and cost saving; the hydrothermal kettle is arranged in the ultrasonic wave generating groove to make inner electrolysis liquid of the hydrothermal kettle lie in an ultrasonic field; thus, the ultrasonic technique, electric deposition technique and hydrothermal technique are combined, and the bonding force of the coatings or the thin films and the base body is enhanced.
Description
Technical field
The present invention relates to a kind of method and device thereof that utilizes ultrasonic wave, hydro-thermal and prepared by electrodeposition coating or film.
Background technology
At present, electrochemical deposition and hydrothermal method be because in preparation film or coatings art outstanding feature and by extensive concern separately, and become the focus of research day by day.The outstanding feature of electrochemical deposition technique is the required equipment less investment, productive expense is low, simple to operate, the utilization rate of raw materials height, process implementing has continuity, easily is automated production, not only can be used for the coated of flat surface, also can on complex surfaces and porous matrix, obtain the coating of uniformity, and the form of the hole of coating, thickness and coated crystal etc. can be controlled all by processing condition; The distinguishing feature of Hydrothermal Preparation film is once to finish in liquid phase, do not need subsequent crystallization heat treatment, thereby curling of having avoided that film may cause in heat treatment process, cracking, grain coarsening, film and defectives such as substrate or atmosphere reaction, and the hydrothermal method required equipment is simple, treatment temp is lower, avoided of the mutually mutual diffusion of processing front and back film with the substrate composition, gained film purity height, homogeneity is good.
Recently, in order fully to fully utilize the advantage of these two kinds of methods, some scholars have carried out correlative study.People such as set up one's own business adopts and uses earlier electrocrystallization Huang, the method that adopts hydrothermal method to handle has then prepared the HA biological coating that purity height, crystal are evenly distributed, carry out that coat-thickness is 50 μ m after the 30min galvanic deposit, and the coating of preparation and the interface bond strength value of titanium alloy reach, and [Huang is set up one's own business about 15MPa, Xu Kewei etc., the electrocrystallization-hydro-thermal of HA coating synthetic and tack and structural stability discussion, Rare Metals Materials and engineering, 1999,28 (3): 140-143]; People such as Liu Fang adopt galvanic deposit-hydro-thermal synthetic bio-ceramic coating, after 700 ℃ of calcination, reach 15.48Mpa with basal body interface bond strength, after alkali lye pre-treatment and under argon shield, be calcined to 900 ℃, interface bond strength reaches 22.39MPa[Liu Fang, Huang Baiyun etc., the galvanic deposit-bio-ceramic coating of hydrothermal synthesis method preparation and the research of basal body interface bond strength, Rare Metals Materials and engineering, 2004,33 (1): 83-86]; People such as Liu Rongfang utilize hydro-thermal-electrodip process to prepare hydroxyapatite coating layer; discovery is under 160 ℃ of hydrothermal conditions; galvanic deposit 4h also is calcined to and can makes about 800 ℃ that coating and high base strength reach [Liu Rongfang etc. about 16.7MPa; the research of hydrothermal electrodeposition hydroxyapatite coating layer; SCI; 2004,25 (2): 304-308].Top method all is to adopt the method for hydrothermal electrodeposition, but can only prepare bio-ceramic coating at present, still can not prepare other ceramic coating or thin-film material.And the coating bonding force of preparation is lower, the bonding force that improves coating and matrix also needs follow-up calcination thermal treatment operations such as (700-900 ℃), coating after calcination is degree of crystallinity and purity is under some influence but also technology is loaded down with trivial details not only, needs to consume a large amount of energy, has increased cost.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of preparation technology simple, cost is low and do not need follow-up thermal treatment, can once directly obtain densification and the good using supersonic, water-heating prepared by electrodeposition coating of bonding force or the method and the device thereof of film.
For achieving the above object, the using supersonic, water-heating prepared by electrodeposition coating that the present invention adopts or the device of film are: comprise the hydro-thermal kettle and be arranged on the electrode that is connected with power supply in the hydro-thermal kettle, the outside of hydro-thermal kettle also is provided with the ultrasonic wave generation trough that is connected with ultrasonic generator, and the ultrasonic wave generation trough is connected with thermostatic bath by drain pipe and liquid returning tube; The upper end of hydro-thermal kettle also is provided with and has manometric hydro-thermal kettle cover, and electrode is installed in water heating kettle by insulation covering and covers; Hydro-thermal kettle internal surface also is provided with water heating kettle Te Fulong liner; Be provided with the temperature-sensing element and the heating unit that are connected with rly. in the thermostatic bath, and also be provided with the submerged pump that is connected with drain pipe in the lower end of thermostatic bath.
For achieving the above object, the preparation method that the present invention adopts is: at first open rly. control heating unit the isothermal liquid in the thermostatic bath is heated, open submerged pump simultaneously, by drain pipe and liquid returning tube isothermal liquid is circulated between thermostatic bath and ultrasonic wave generation trough, work by the temperature-sensing element relay, the registration for the treatment of thermometer show isothermal liquid reach required preparation coating or film temperature and stable after, be incubated; Open the hydro-thermal kettle cover, electrolytic solution is inserted in the hydro-thermal kettle, be connected on the electrode after with sample holder sample being clipped; The hydro-thermal kettle is placed the ultrasonic wave generation trough, and start ultrasonic generator thereupon, the ultrasonic power of adjusting ultrasonic generator and frequency are to the predetermined value of required preparation coating or film; Treat tensimeter show the pressure of hydro-thermal kettle reach the predetermined value of required preparation coating or film and registration stable after, power-on begins to carry out galvanic deposit; After being deposited into the scheduled time of the coating of required preparation or film, at first powered-down is closed ultrasonic generator again, makes ultrasonic system out of service, and last closed relay and submerged pump make the circulation constant temperature system out of service; After treating that the hydro-thermal kettle is cooled to room temperature, open the hydro-thermal kettle cover, take out sample, promptly can obtain having prepared film or coating of material sample.
Because the present invention carries out temperature control by thermostatic bath to the hydro-thermal kettle, the coating or the film of the direct synthesis of densified of super critical condition of hydrothermal technique, utilize galvanic deposit to control sedimentary thickness, avoided later stage thermal treatment, simplified preparation technology, saved cost, and the hydro-thermal kettle placed in the ultrasonic wave generation trough, the intravital electrolytic solution of water heating kettle is in the ultrasonic wave field, thereby with ultrasonic technology, galvanic deposit and hydrothermal technique merge together, improved the bonding force of coating or film and matrix, the bonding force of coating or film and matrix is far longer than the 2-5MPa of ultrasonic galvanic deposit and the 1-3MPa of hydrothermal electrodeposition generally greater than 10Mpa.Can once directly obtain densification and the good coating of bonding force, coating does not need follow-up thermal treatment, and the preparation method is simple, cost is lower, can make full use of the above-mentioned advantage of galvanic deposit and hydrothermal technique, can solve the interface bond strength problem when Front-coating mirror and matrix again to a certain extent.
Description of drawings
Accompanying drawing is an one-piece construction synoptic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Referring to accompanying drawing, be provided with the hydro-thermal kettle 9 and the hydro-thermal kettle cover 8 that has tensimeter 7 of electrolytic solution 20 in the present invention includes, hydro-thermal kettle 9 internal surfaces also are provided with water heating kettle Te Fulong liner 10, electrode 4 is installed on the hydro-thermal kettle cover 8 and with power supply 5 by insulation covering 6 and is connected, the outside of hydro-thermal kettle 9 also is provided with the ultrasonic wave generation trough 2 that is connected with ultrasonic generator 1, be provided with isothermal liquid 19 in the ultrasonic wave generation trough 2, ultrasonic wave generation trough 2 is connected with thermostatic bath 15 by drain pipe 12 and liquid returning tube 18, and be provided with temperature-sensing element 13 and heating unit 17 that is connected with rly. 11 and the thermometer 14 that is used to observe isothermal liquid 19 temperature in the thermostatic bath 15 in thermostatic bath 15, the lower end of thermostatic bath 15 also is provided with the submerged pump 16 that is connected with drain pipe 12.
Preparation method of the present invention is as follows:
1) isothermal liquid of at first opening in 17 pairs of thermostatic baths of rly. 11 control heating units 15 19 heats, open submerged pump 16 simultaneously, make isothermal liquid 19 in thermostatic bath 15 and 2 circulations of ultrasonic wave generation trough by drain pipe 12 and liquid returning tube 18, work by temperature-sensing element 13 relays 11, the registration for the treatment of thermometer 14 show isothermal liquid 19 reach required preparation coating or film temperature and stable after, be incubated;
2) prepare required electrolytic solution 20 according to the composition and the correlation parameter of coating or film then;
3) with the spanner hydro-thermal kettle cover 8 of outwarding winding, the electrolytic solution 20 for preparing is before moved in the hydro-thermal kettle 9, be connected on the electrode 4 after with sample holder 3 sample 21 being clipped;
4) hydro-thermal kettle 9 is placed ultrasonic wave generation trough 2, and start ultrasonic generator 1 thereupon, the ultrasonic power of adjusting ultrasonic generator 1 and frequency are to the predetermined value of required preparation coating or film;
5) treat tensimeter 7 show the pressure of hydro-thermal kettlies 9 reach the predetermined value of required preparation coating or film and registration stable after, power-on 5 begins to carry out galvanic deposit;
5) be deposited into the scheduled time of the coating of required preparation or film after, at first powered-down 5, close ultrasonic generator 1 again, make ultrasonic system out of service, last closed relay 11 and submerged pump 16 make the circulation constant temperature system out of service;
6) treat that hydro-thermal kettle 9 is cooled to room temperature after, open hydro-thermal kettle cover 8, take out sample 21, promptly can obtain having prepared film or coating of material sample.
The present invention makes cathode and anode all place reaction kettle body 9 inside by the galvanic deposit electrode used therein appropriately is connected with the hydro-thermal kettle cover, thereby with galvanic deposit and hydrothermal technique is ingenious combines together; By water-bath or oil bath (specifically deciding) temperature is controlled by the required temperature of reaction; Hydro-thermal kettle 9 is placed in the ultrasonic wave generation trough 2, the electrolytic solution 20 of hydro-thermal kettle 9 is in the ultrasonic wave field, thereby ultrasonic technology, galvanic deposit and hydrothermal technique are merged in the present invention.
The present invention has improved the bonding force of coating or film and matrix by ultrasonic wave, the coating or the film of the direct synthesis of densified of super critical condition of hydrothermal technique, utilize galvanic deposit to control sedimentary thickness, avoided later stage thermal treatment, simplified preparation technology, save cost, finally prepared high-quality coating or thin-film material.
Claims (5)
1. the device of using supersonic, water-heating prepared by electrodeposition coating or film, comprise hydro-thermal kettle [9] and be arranged on the electrode [4] that is connected with power supply [5] in the hydro-thermal kettle [9], it is characterized in that: the outside of hydro-thermal kettle [9] also is provided with the ultrasonic wave generation trough [2] that is connected with ultrasonic generator [1], and ultrasonic wave generation trough [2] is connected with thermostatic bath [15] by drain pipe [12] and liquid returning tube [18].
2. the device of using supersonic, water-heating prepared by electrodeposition coating according to claim 1 or film, it is characterized in that: the upper end of said hydro-thermal kettle [9] also is provided with the hydro-thermal kettle cover [8] that has tensimeter [7], and electrode [4] is installed on the hydro-thermal kettle cover [8] by insulation covering [6].
3. the device of using supersonic, water-heating prepared by electrodeposition coating according to claim 1 or film is characterized in that: said hydro-thermal kettle [9] internal surface also is provided with water heating kettle Te Fulong liner [10].
4. the device of using supersonic, water-heating prepared by electrodeposition coating according to claim 1 or film, it is characterized in that: be provided with the temperature-sensing element [13] and the heating unit [17] that are connected with rly. [11] in the said thermostatic bath [15], and also be provided with the submerged pump [16] that is connected with drain pipe [12] in the lower end of thermostatic bath [15].
5. a device that adopts claim 1 described using supersonic, water-heating prepared by electrodeposition coating or film prepares the method for coating or film, it is characterized in that:
1) at first opens rly. [11] control heating unit [17] to the heating of the isothermal liquid [19] in the thermostatic bath [15], open submerged pump [16] simultaneously, by drain pipe [12] and liquid returning tube [18] isothermal liquid [19] is circulated between thermostatic bath [15] and ultrasonic wave generation trough [2], work by temperature-sensing element [13] relay [11], the registration for the treatment of thermometer [14] show isothermal liquid [19] reach required preparation coating or film temperature and stable after, be incubated;
2) open hydro-thermal kettle cover [8], electrolytic solution [20] is inserted in the hydro-thermal kettle [9], be connected on the electrode [4] after with sample holder [3] sample [21] being clipped;
3) hydro-thermal kettle [9] is placed ultrasonic wave generation trough [2], and start ultrasonic generator [1] thereupon, the ultrasonic power of adjusting ultrasonic generator [1] and frequency are to the predetermined value of required preparation coating or film;
4) treat tensimeter [7] show the pressure of hydro-thermal kettle [9] reach the predetermined value of required preparation coating or film and registration stable after, power-on [5] begins to carry out galvanic deposit;
5) be deposited into the scheduled time of the coating of required preparation or film after, at first powered-down [5] is closed ultrasonic generator [1] again, makes ultrasonic system out of service, last closed relay [11] and submerged pump [16] make the circulation constant temperature system out of service;
6) treat that hydro-thermal kettle [9] is cooled to room temperature after, open hydro-thermal kettle cover [8], take out sample [21], promptly can obtain having prepared film or coating of material sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100960878A CN100396823C (en) | 2005-09-29 | 2005-09-29 | Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100960878A CN100396823C (en) | 2005-09-29 | 2005-09-29 | Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology |
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| CN1766175A CN1766175A (en) | 2006-05-03 |
| CN100396823C true CN100396823C (en) | 2008-06-25 |
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| CNB2005100960878A Expired - Fee Related CN100396823C (en) | 2005-09-29 | 2005-09-29 | Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology |
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| CN102350288B (en) * | 2011-08-22 | 2013-12-18 | 浙江工业大学 | Ultrasonic-hydro-thermal coupling apparatus for preparing nano-material |
| CN103173842B (en) * | 2013-02-25 | 2016-03-30 | 上海大学 | The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment |
| CN104868111A (en) * | 2015-03-27 | 2015-08-26 | 陕西科技大学 | Preparation method of Ce doped Li4Ti5O12 lithium ion battery cathode material |
| CN106906501B (en) * | 2017-03-30 | 2018-12-28 | 江苏理工学院 | A kind of overcritical electric deposition device of ultrasonic wave added |
| CN108998819B (en) * | 2018-05-29 | 2019-08-02 | 深圳大学 | The preparation method of microwave hydrothermal electro-deposition system and calcium phosphorus biological coating |
| CN111334843B (en) * | 2020-04-26 | 2021-09-14 | 重庆理工大学 | Preparation device for metallurgical bonding coating on inner wall of metal pipe |
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Assignee: Zhuhai matsuda electrician Co., Ltd Assignor: Shaanxi University of Science and Technology Contract record no.: 2010440000510 Denomination of invention: Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology Granted publication date: 20080625 License type: Exclusive License Open date: 20060503 Record date: 20100518 |
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