CN1050389C - Energy control method for plasma enhanced electrochemical formation of cermet - Google Patents
Energy control method for plasma enhanced electrochemical formation of cermet Download PDFInfo
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Abstract
The present invention provides a control method of a ceramic technique of a plasma-body enhanced electrochemical surface, which is suitable for large-scale industrial production. In the control method of a ceramic technique of a plasma-body enhanced electrochemical surface, the plasma arc discharge of the surface of a metal base body as an anode is generated by electric energy under the existing electrolyte solution and a corresponding technological condition, and the anode is electrochemically oxidized. When a film layer with a ceramic structure is formed, a conducting angle of controllable silicon and a conducted cycle number in unit time are controlled by a three-phase bridge type interruption cycle full-control rectified method, energy (sintered energy) acted on a micro plasma body of the surface of a work piece can be reasonably controlled, and the control method of a ceramic technique of a plasma-body enhanced electrochemical surface avoids under-sintering phenomenon, over-sintering phenomenon and ablating phenomenon in a sintering process and also simultaneously reduces the harmonic pollution of a network.
Description
The present invention relates to the anodised method of metal material surface, particularly relate to a kind of plasma intensified electrochemical surface potteryization energy control method.
Metal and alloy surface potteryization improve its performance to further widening the use range of metallic substance, replace precious materials with cheap material, improve the processability of stupalith, and it is significant to reduce cost.
The plasma intensified electrochemical surface potteryization is on the basis of common anode oxidation technology, utilize high density energy that plasma body has to activate and strengthen the electrochemical reaction on anode and reaction product carried out sintering, thereby obtain to have a kind of method of the pottery coating of superperformance on the valve metal surface.
Chinese patent 95114880.x has provided and a kind of valve metal and alloy has been carried out the method for plasma intensified electrochemical surface potteryization, and this method adopts voltage 100-400V, current density 0.5-20A/dm in the electrolyte solution of fixing component
2Direct supply on anode (workpiece) surface, prepare the potteryization coating.But there is the problem of following several respects in this patented method in large-scale commercial process:
1, adopt pure direct supply, idle power consumption is excessive in the technological process, and promptly Zhuan Zhi powerfactorcos is lower, only is 0.3-0.7.
2, owing to adopt silicon controlled rectifier, very easily produce higher harmonic, seriously polluted to electrical network at source end (AC side).
3, because the control of energy mode is fixed, make the ceramic film sintering process be prone to " underburnt ", " burning " reaches " ablation " phenomenon.
" underburnt " is the sintering energy shortage, the ceramic layer structure vegetables pine of generation, and phase transition is not thorough, and grade is low, thereby makes a kind of phenomenon of its degradation.The underburnt overwhelming majority takes place be because after the blocking layer generates, along with the progressive additive of ceramic layer, the sintering energy is not enough so that whole ceramic film generation sintering phase transformation and causing.Avoiding the underburnt most effectual way is in time to increase the sintering energy along with ceramic layer thickness increases gradually in technological process.
" burning " is that the ceramic surface roughness of the higher generation of sintering energy density increases the phenomenon that rete fragility increases.
" ablation " is that the sintering energy density is too high, makes ceramic layer produce liquid phase sintering, causes the matrix fusing, makes and excessively concentrates and the breakoff phenomenon of generation in melting area self-energy density.
" burning " reaches " ablation " all is because the sintering energy density is higher than due to the normal value, and the best means of stopping burning and ablation is a strict control sintering energy in whole technological process.
The objective of the invention is to overcome the above-mentioned defective of prior art, provide a kind of idle power consumption little (power factor height), low to the electric network pollution degree, the large-scale commercial production ionic medium that is applicable to of Energy Controllable strengthens the control method of electrochemical surface ceramic technology.
The present invention adopts identical electrolyte solution and the corresponding technological conditions described in the Chinese patent 95114880.x, make as anodic metal base surface plasma arc light discharge by electric energy, carry out electrochemical anodic oxidation, formation has the rete of ceramic structure, adopt the method for the interrupted cycle full-controlled rectifier of three-phase bridge, the cycle of conducting is reasonably controlled the energy (being the sintering energy) that acts on the workpiece surface microplasma in rationally control silicon controlled conduction angle and unit time.
The concrete technology of the energy control method of plasma intensified electrochemical surface potteryization of the present invention is: in electrolyte solution, make as the basic surface plasma arc discharge of anodic metal by electric energy, carry out electrochemical anodic oxidation, formation has the rete of ceramic structure, wherein, described electrolyte solution is with Sodium hexametaphosphate 99 (10-50g/l), boric acid and/or borax (5-20g/l) are main, also contain at least a sodium orthophosphate that is selected from, sodium sulfate, water glass, ammonium meta-vanadate, sodium metavanadate, Sodium chromate, sodium wolframate, rose vitriol, single nickel salt, ferric sulfate, manganous sulfate, the oxysalt of chromium sulphate, and can select adding to be selected from calcium, zinc, cobalt, the acetate of nickel, silicofluoric acid, Potassium monofluoride, the additive of ethylenediamine tetraacetic acid (EDTA), arc discharge voltage is 100-400V, and current density is 0.5-20A/dm
2The electrolyte solution temperature is 10-50 ℃, it is characterized in that adopting the interrupted cycle full-controlled rectifier of three-phase bridge, the cycle of conducting in control silicon controlled conduction angle and unit time, make the microplasma energy (being the sintering energy) that acts on workpiece surface controlled, selected conducting cycle is respectively 37.5/second, 75/second, 150/second, 300/second, and in whole technological process, the conducting cycle is selected and controlled according to the different span of control of sintering energy, the silicon controlled conduction angle is 0-170 °, and, make the sintering energy of ceramic layer be controlled at 50W/dm by the silicon controlled conduction angle with to the energy of the reasonable switching controls plasma body of described four kinds of conducting cycles
2S-600W/dm
2S.
The electrolyte solution that method of the present invention is used and corresponding other processing condition are described identical with Chinese patent 95114880.x, the inventive method is to have given prominence to the energy control method in the oxidizing process process on the technology basis of this patent, " underburnt ", " burning " having avoided occurring in sintering process reach " ablation " phenomenon, when guaranteeing to obtain good ceramic phase structure rete, the power factor that has improved the equipment work process reaches 0.6-0.9, has reduced the harmonic pollution to network.
Narrate concrete control below respectively to ceramic film sintering energy under the different process kind.
1, the energy control in the porcelain white porcelain membrane prepare process
Pressing Chinese patent 95114880.x electrolyte solution forms and processing condition, the conducting cycle is 300/second and 150/second in selection unit's time, early stage, 10-20% got 300/second in the process time, thyristor operating angle is 0-60 °, get 150/second in the later stage 80-90% process time, thyristor operating angle is 60 °-170 °.Control sintering energy is 90-150W/dm
2S, whole technological process powerfactorcos is 0.6-0.9, the ceramic film of preparing does not have underburnt, burning and ablation phenomen.
2, the control of the energy in the blue look ceramic membrane preparation process
Pressing the electrolyte solution of Chinese patent 95114880.x forms and corresponding processing condition, the conducting cycle is 75/second and 150/second in selection unit's time, early stage, 10-20% got 150/second in the process time, thyristor operating angle 0-120 °, get 75/second in the later stage 80-90% process time, thyristor operating angle 100-170 °, control sintering energy is 120-240W/dm
2S.Whole technological process powerfactorcos is 0.65-0.90, and the ceramic film of preparing does not have underburnt, burning and ablation phenomen.
3, the control of the energy in the cream-coloured ceramic membrane preparation process
The conducting cycle is 150/second and 75/second in selection unit's time, and early stage, 10-15% in the process time was 150/second, got 75/second in the later stage 85-90% process time, and control sintering energy is 110-230W/dm
2S, whole technological process powerfactorcos is 0.7-0.90.
4, the control of the energy in the dark pink ceramic membrane preparation process
The conducting cycle is 150/second and 75/second in selection unit's time, and early stage, 5-15% in the process time was 150/second, was 75/second in the later stage 85-95% time, and control sintering energy is 50-300W/dm
2S, whole technological process powerfactorcos is 0.7-0.90.
5, the control of the energy in the coffee-like ceramic membrane preparation process
The conducting cycle is 150/second, 75/second in selection unit's time, with 300/second, early stage, 10-15% in the process time was 150/second, and mid-term, 55-65% in the process time was 75/second, in the later stage 20-30% process time be 300/second, control sintering energy is 220-440W/dm
2S, whole technological process powerfactorcos is 0.7-0.90.
6, yellow fraction to the energy in the yellow ceramic membrane preparation process is controlled
The conducting cycle is 75/second and 150/second in selection unit's time.Early stage, 10-30% in the process time was 75/second, was 150/second in the later stage 70-90% process time, and control sintering energy is 140-320W/dm
2S, whole technological process powerfactorcos is 0.7-0.90.
7, sintering control of energy in the coppery rete preparation process modelled after an antique
The conducting cycle is 300/second, 150/second and 75/second in selection unit's time.Early stage, 10-15% in the process time was 300/second, and mid-term, 70-75% in the process time was 150/second, was 75/second in the later stage 15-20% process time, and control sintering energy is 110-260W/dm
2S, whole technological process powerfactorcos is 0.6-0.9.
8, sintering control of energy in the grey ceramic film preparation process
The conducting cycle is 300/second, 75/second and 150/second in selection unit's time.Early stage, 5-10% in the process time was 300/second, and mid-term, 70-75% in the process time was 75/second, was 150/second in the later stage 10-20% process time, and control sintering energy is 80-150W/dm
2S, whole technological process powerfactorcos is 0.6-0.9.
9, sintering control of energy in the hard ceramic rete preparation process
The conducting cycle is 37.5/second, 75/second and 150/second in selection unit's time.In 45% process time of early stage is 37.5/second, and mid-term, 20-45% in the process time was 75/second, was 150/second in the later stage 10-35% process time, and control sintering energy is 90-600W/dm
2S.
By the present invention, under commercial production conditions, obtained good uniformity, hole is low, and with the substrate combinating strength height, nothing " underburnt ", " burning " reach the pottery rete of " ablation " phenomenon.
Method of the present invention goes for the suitability for industrialized production of the valve metal workpiece of virtually any size, shape and structure.
Further specify the present invention below by embodiment.
Embodiment 1
In the suitability for industrialized production oxidation trough that is of a size of 8000 * 1400 * 2200 (mm), inject the given porcelain white electrolyte solution 20000kg of Chinese patent 95114880.x, the LD31 aluminium alloy of cleaning is communicated with power supply together with anchor clamps (workpiece surface amasss 30m
2).Make workpiece make anode, make negative electrode, adopt pressurized air and spray to stir to tank liquor, and control its temperature at 10 ℃ with stainless steel plate.Adopt 300/second cycles to regulate the silicon controlled conduction angle, make it in 0-60 ° of scope, to change.Control sintering energy density is (110 ± 5%) W/dm
2S.Cycle with 150/second is regulated the silicon controlled conduction angle again after 3 minutes, makes it to change in 60-120 ° of scope, and needing control sintering energy density this moment is (120 ± 5%) W/dm
2S.After 17 minutes, stop, taking out workpiece can obtain superperformance after rinsing, oven dry pottery rete.After testing, α-Al in this rete
2O
3+ SiO
2Content surpass 95%, show that its ceramic phase sintering is reasonable, cos φ value is 0.6 in the time period in the early stage in the technological process, is 0.85-0.90 in the time period in later stage.Its wear-resisting evaluation, blocks 9 grades of this experiments, Hv:410kg/mm at 300 seconds sandblast time
2(5g).
Embodiment 2
In the suitability for industrialized production oxidation trough that is of a size of 8000 * 1400 * 2200 (mm), inject the given blue look ceramic membrane electrolyte solution 20000kg of Chinese patent 95114880.x, the porcelain that will prepare white LD31 Al alloy parts (surface-area 20m by the method for embodiment 1
2) after cleaning, put into this oxidation trough, workpiece connects power anode, and negative electrode links to each other with stainless steel polar plate, and makes solution keep static, and temperature is 20 ℃.With 150/second cycle energisings 90 seconds, thyristor operating angle was 0-100 °, and control sintering energy density is (135 ± 5%) W/dm
2S sprays stirring to electrolyte solution then, continues energising 180 seconds with 75/second cycles, and thyristor operating angle is 100-170 °, and control sintering energy is (145 ± 5%) W/dm
2S, early stage, cos φ was 0.90, gained potteryization film after testing, the transformation mutually of ceramic layer is thorough, is c-Al
2O
3And SiO
2, CoO, wear-resisting evaluation, 340 seconds sandblast time, block this experiment 9 grades, Hv:440kg/mm
2(5g).
Embodiment 3
In the suitability for industrialized production oxidation trough that is of a size of 8000 * 1400 * 2200 (mm), inject the given grey ceramic membrane electrolyte solution 20000kg of Chinese patent 95114880.x, workpiece is surface-area 24m
2Fine aluminium sheet material, after cleaning, insert in the groove, workpiece is made anode, negative electrode is a stainless steel plate, stirs, temperature is 35 ℃, adopts 300/second cycles, conduction angle is 0-60 °, 2 minutes time, controlling energy density is (120 ± 5%) W/dm
2S adopts 75/second cycles then, conduction angle 50-100 °; 12 minutes time, the control energy density is (135 ± 5%) W/dm
2S.At last, adopt 150/second cycles, conduction angle 100-120 °, 5 minutes time, the control energy density is (140 ± 5%) W/dm
2S, early stage, cos φ was 0.6, and mid-term, cos φ was 0.8, and later stage cos φ is 0.85, and gained potteryization film thing phase composite after testing is α-Al
2O
3+ and SiO
2+ NiO.
Embodiment 4
In the suitability for industrialized production oxidation trough that is of a size of 2000 * 2000 * 1500 (mm), inject the given hard ceramic layer electrolyte solution 5000kg of Chinese patent 95114880.x, workpiece is surface-area 10m
2Ti
6Al
4V alloy is inserted in the groove behind clear Xian, and workpiece is an anode, and negative electrode is the stainless steel plate plate, stirs, and 35 ℃ of tank liquor temperatures adopt 150/second cycle energisings 10 minutes, and conduction angle 0-100 °, control sintering energy is (170 ± 20%) W/dm
2S adopts 75/second cycle to switch on then 45 minutes, and conduction angle 100-140 °, control sintering energy is (190 ± 30%) W/dm
2S adopts 37.5/second cycles at last, switched on 45 minutes, and conduction angle 140-170 °, control sintering energy (250 ± 50%) W/dm
2S.The gained potteryization film thing structure that combines after testing is TiO
2+ SiO
2+ W
2O
3, wear-resisting evaluation, 1500 seconds sandblast time, Hv:1300kg/mm
2(5g).Block 9 grades of this experiments.
Such scheme only provides as embodiment, and does not limit the present invention in any way, and those skilled in the art can carry out the various improvement that change over to the present invention, but does not all break away from the protection domain of essence of the present invention and claim.
Claims (10)
1, plasma intensified electrochemical surface potteryization energy control method, this method is included in the electrolyte solution, make as anodic metal base surface plasma arc light discharge by electric energy, carry out electrochemical anodic oxidation, formation has the rete of ceramic structure, wherein, described electrolyte solution is with Sodium hexametaphosphate 99 (10-50g/l), boric acid and/or borax (5-20g/l) are main, also contain at least a sodium orthophosphate that is selected from, sodium sulfate, water glass, ammonium meta-vanadate, sodium metavanadate, Sodium chromate, sodium wolframate, rose vitriol, single nickel salt, ferric sulfate, manganous sulfate, the oxysalt of chromium sulphate, and can select adding to be selected from calcium, zinc, cobalt, the acetate of nickel, silicofluoric acid, Potassium monofluoride, the additive of ethylenediamine tetraacetic acid (EDTA), arc discharge voltage is 100-400V, and current density is 0.5-20A/dm
2The electrolyte solution temperature is 10-50 ℃, it is characterized in that adopting the interrupted cycle full-controlled rectifier of three-phase bridge, the cycle of conducting in control silicon controlled conduction angle and unit time, make the microplasma energy (being the sintering energy) that acts on workpiece surface controlled, selected conducting cycle is respectively 37.5/second, 75/second, 150/second, 300/second, and in whole technological process, the conducting cycle is selected and controlled according to the different span of control of sintering energy, the silicon controlled conduction angle changes in 0-170 °, and sintering energy span of control is 50W/dm
2S-600W/dm
2S.
2, the described method of claim 1, it is characterized in that selecting the conducting cycle is 300/second and 150/second, control sintering energy is 90-150W/dm
2S, wherein 300/second account for the 10-20% time, 150/second times that account for 80-90%.
3, the described method of claim 1, it is characterized in that selecting the conducting cycle is 75/second and 150/second, control sintering energy is 120-240W/dm
2S, wherein 150/second account for the 10-20% time, 75/second times that account for 80-90%.
4, the described method of claim 1, it is characterized in that selecting the conducting cycle is 150/second and 75/second, control sintering energy is 110-230W/dm
2S, wherein 150/second account for the 10-15% time, 75/second times that account for 85-90%.
5, the described method of claim 1, it is characterized in that selecting the conducting cycle is 150/second and 75/second, control sintering energy is 50-300W/dm
2S, wherein 150/second account for the 5-15% time, 75/second times that account for 85-95%.
6, the described method of claim 1 is characterized in that selecting 75/second of conducting cycles and 150/second and 300/second, and control sintering energy is 200-440W/dm
2S, the 10-15% time its mid-early stage is 150/second, and the 55-65% time in mid-term is 75/second, and the later stage 20-30% time is 300/second.
7, the described method of claim 1, it is characterized in that selecting the conducting cycle is 75/second and 150/second, control sintering energy is 140-320W/dm
2S, 75/second times that account for 10-30% wherein, 150/second times that account for 70-90%.
8, the described method of claim 1, it is characterized in that selecting the conducting cycle is 300/second, 150/second and 75/second, control sintering energy is 110-260W/dm
2S, the 10-15% time its mid-early stage is 300/second, and the 70-75% time in mid-term is 150/second, and the later stage 15-20% time is 75/second.
9, the described method of claim 1, it is characterized in that selecting the conducting cycle be 300/second and 75/second, 150/second, control sintering energy is 80-150W/dm
2S, the 5-10% time its mid-early stage is 300/second, and the 70-75% time in mid-term is 75/second, and the later stage 10-20% time is 150/second.
10, the described method of claim 1, it is characterized in that selecting the conducting cycle is 37.5/second and 75/second and 150/second, control sintering energy is 90-600W/dm
2S, its 45% time of mid-early stage is 37.5/second, and the 20-45% time in mid-term is 75/second, and the later stage 10-35% time is 150/second.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97104035A CN1050389C (en) | 1997-04-21 | 1997-04-21 | Energy control method for plasma enhanced electrochemical formation of cermet |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97104035A CN1050389C (en) | 1997-04-21 | 1997-04-21 | Energy control method for plasma enhanced electrochemical formation of cermet |
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|---|---|
| CN1163323A CN1163323A (en) | 1997-10-29 |
| CN1050389C true CN1050389C (en) | 2000-03-15 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1769526B (en) * | 2005-12-02 | 2010-08-25 | 中国科学院物理研究所 | Method and device for internal wall ceramic treatment of steel and iron pipe casting |
| KR101195458B1 (en) * | 2009-04-22 | 2012-10-30 | 한양대학교 에리카산학협력단 | Method for treating the surface of metal |
| CN101705511B (en) * | 2009-11-30 | 2011-04-20 | 哈尔滨工业大学 | Method for preparing alumina-ferric oxide ceramic membrane with controllable solar absorptance |
| CN103173838B (en) * | 2013-04-11 | 2015-07-01 | 江西科技师范大学 | Magnesium alloy micro-arc oxidation electrolyte and micro-arc oxidation method |
| CN106435681B (en) * | 2016-10-23 | 2018-11-16 | 深圳合一技术科技发展有限公司 | The production method and device of aluminium oxide nano layer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1504292A1 (en) * | 1987-08-17 | 1989-08-30 | Московский Институт Нефти И Газа Им.И.М.Губкина | Apparatus for microarc oxidizing of rectifier metals and their alloys |
| SU1624060A1 (en) * | 1989-03-10 | 1991-01-30 | Московский авиационный технологический институт им.К.Э.Циолковского | Apparatus for microdischarge oxidation of rectifier metals and alloys |
| CN1115793A (en) * | 1995-04-18 | 1996-01-31 | 哈尔滨环亚微弧技术有限公司 | Plasma enhanced electrochemical surface ceramization method and product |
-
1997
- 1997-04-21 CN CN97104035A patent/CN1050389C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1504292A1 (en) * | 1987-08-17 | 1989-08-30 | Московский Институт Нефти И Газа Им.И.М.Губкина | Apparatus for microarc oxidizing of rectifier metals and their alloys |
| SU1624060A1 (en) * | 1989-03-10 | 1991-01-30 | Московский авиационный технологический институт им.К.Э.Циолковского | Apparatus for microdischarge oxidation of rectifier metals and alloys |
| CN1115793A (en) * | 1995-04-18 | 1996-01-31 | 哈尔滨环亚微弧技术有限公司 | Plasma enhanced electrochemical surface ceramization method and product |
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