CN103361594A - Surface carburization and nitridation treatment method for steel workpiece - Google Patents

Surface carburization and nitridation treatment method for steel workpiece Download PDF

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Publication number
CN103361594A
CN103361594A CN2013103423431A CN201310342343A CN103361594A CN 103361594 A CN103361594 A CN 103361594A CN 2013103423431 A CN2013103423431 A CN 2013103423431A CN 201310342343 A CN201310342343 A CN 201310342343A CN 103361594 A CN103361594 A CN 103361594A
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nicarbing
quenching
work piece
piece surface
steel work
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杉山辉阳
野口奉夫
刘其城
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HUNAN TECHNO THERMAL TREATMENT Co Ltd
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HUNAN TECHNO THERMAL TREATMENT Co Ltd
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Abstract

The invention discloses a surface carburization and nitridation treatment method for a steel workpiece, which comprises the following steps: placing a steel workpiece into a heating chamber; vacuumizing, then introducing nitrogen gas to ensure that the steel workpiece is in a nitrogen gas atmosphere, and controlling the atmosphere pressure in the furnace to be 100 Torr or above; then heating to enable the steel workpiece to reach a carburization and nitridation temperature, keeping the aforementioned pressure in the furnace, and alternately introducing unsaturated hydrocarbon gas and ammonia gas to perform high-temperature carburization and nitridation; after the high-temperature carburization and nitridation is completed, cooling to a quenching temperature, and then performing quenching heat preservation and quenching cooling; and finally, completing the surface carburization and nitridation treatment of the steel workpiece. The method disclosed by the invention has the advantages of simple equipment, low investment, high heating efficiency and good product quality.

Description

A kind of steel work piece surface nicarbing treatment process
Technical field
The present invention relates to a kind of surface-hardening treatment method of mechanical part, relate in particular to a kind of surface cementation nitridation treatment method of mechanical part.
Background technology
Vacuum carburizing in the existing carburizing treatment method is after allowing processed steel workpiece heat to the carburizing temperature of regulation in vacuum oven and making it to keep soaking, the saturated hydrocarbon (stable hydrocarbon) of the gaseous states such as the methane that past heating chamber importing is used as carburizing gas, propane, butane, make again its thermolysis, make consequent activated carbon invade surface as the steel workpiece of object being treated.Compare with existing gas cementation technology, vacuum carburizing have process, need not between can high temperature, short time rotten stove, atmosphere surrounding simple and convenient management, substantially do not occur the particle oxidation, can carry out the advantage such as intermittent operation.
On the other hand, use saturated hydrocarbon gas easily to cause the generation of impurity as the vacuum carburizing of carburizing medium, therefore, employing unsaturated hydrocarbon gas (unsaturated hydrocarbons such as the chain such as acetylene, ethene) occurs and replaced the stable hydrocarbon such as methane, propane as the vacuum carburizing of carburizing medium.Yet, because the chemical stability of the chain unsaturated hydrocarbons such as acetylene, ethene is not as saturated hydrocarbon, the thermolysis of unsaturated hydrocarbon gas will be stronger than carburization reaction, and can produce impurity equally, therefore, traditional idea thinks, unsaturated hydrocarbon gas is not suitable for as carburizing medium.And as the unsaturated hydrocarbon gas of carburizing medium, add the ammonia of supplying with as the nitrogen source, although can realize simultaneously in the work piece surface carburizing and infiltrate nitrogen, become technically more difficult because the furnace pressure in the vacuum carburizing is crossed low as the supply of the ammonia in nitrogen source; And, under vacuum condition, after nicarbing, cooling to quenching temperature and remain on this interval of quenching temperature, escaping phenomena can occur in the nitrogen of infiltration, and this is so that process when carburizing and nitrogenize and become more difficult in industrial application.
In addition, the vacuum carbonitriding method is heating chamber to be set under the vacuum state below the 1kPa heat and carburizing, therefore body of heater need to have the seal construction of height, this is when having improved equipment cost, because convection current does not occur in the atmosphere gas in the stove, when packing stove into high-density within, workpiece adds man-hour, not only heat-up rate is slower, and the workpiece thermal radiation absorption heat by heating element only, the difference of workpiece present position is easy to cause the phenomenon of temperature inequality to occur during shove charge.
How to develop the treatment process that a kind of net effect better carries out nicarbing simultaneously, this becomes the problem that those skilled in the art face for a long time.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provides that a kind of equipment is simple, input is little, intensification efficient is high, the steel work piece surface nicarbing treatment process of good product quality.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of steel work piece surface nicarbing treatment process, may further comprise the steps: the steel workpiece is packed in the heating chamber, vacuumize first and pass into again nitrogen, the steel workpiece is in the nitrogen atmosphere, furnace atmosphere pressure is controlled at more than the 110Torr, then heating makes the steel workpiece reach the nicarbing temperature, keep pressure in the aforementioned stove, and pass at intervals unsaturated hydrocarbons gas and ammonia carries out the high temperature carburizing nitrogenize, (cooling herein comprises that holding temperature is constant to cool to quenching temperature after the high temperature carburizing nitrogenize is finished, be that high temperature carburizing nitrogenize and quenching and preserving heat can be carried out under uniform temp), then carry out quenching and preserving heat and quench cooled, finish at last the nicarbing of steel work piece surface is processed.(still needing to pass into unsaturated hydrocarbons gas and ammonia in diffusion, cooling and insulation quenching stage).
In the technique scheme that the present invention proposes, by supplying with at intervals carburizing chain unsaturated hydrocarbons gas, the carbon element of work piece surface is infiltrated and the internal divergence process of (infiltrations) surperficial carbon element can alternately be carried out repeatedly, so just can effectively overcome since carbon concentration too high the sedimentation problem of cementite coal of rapid generation; By supplying with at intervals nitrogenize ammonia (nitrogen source), the nitrogen infiltration of work piece surface and the internal divergence process of (infiltration) surperficial nitrogen also can alternately be carried out repeatedly, compare continuous supplying to situation, because being intermittent, ammonia feeds, the concentration of ammonia can raise at short notice like this, nitriding velocity also can promote, and the situation of nitrogenize inequality can obviously reduce.In addition, the time point, the timed interval and the intake that pass into of ammonia needn't be in full accord with chain unsaturated hydrocarbons gas.
In the technical scheme of the invention described above, described high temperature carburizing nitridation process preferably includes the nicarbing stage of leading portion and the diffusion phase of back segment.In this preferred technical scheme, after finishing, the high temperature carburizing nitrogenize stage namely is transferred to follow-up diffusion phase, and cool to again quenching temperature and carry out follow-up quenching and preserving heat and quench cooled.As for the division of nicarbing stage and diffusion phase, usually diffusion phase consuming time can be set as consuming time roughly the same with the nicarbing stage, also can be with the consuming time suitable shortening of diffusion phase.Certainly, in the more shallow situation of workpiece case depth of design, also diffusion phase can be set, directly after the nicarbing stage finishes, cool to quenching temperature.
Above-mentioned steel work piece surface nicarbing treatment process, in the whole process that described nicarbing is processed, furnace atmosphere pressure preferably is controlled at 500Torr~800Torr, can be chosen in especially under the standard atmospheric pressure (i.e. 760 Torr), the furnace atmosphere pressure measure of control of this moment are the most simple and convenient, process efficiency is higher, and process costs is lower.Certainly, this pressure control condition is not necessary, is higher or lower than this preferred pressure span of control, can not bring technical any obstacle yet.In addition, we also can be in the whole process that nicarbing is processed be controlled at the atmosphere pressure in each stage roughly in the suitable pressure values scope, when workpiece is transplanted on quenching chamber from heating chamber, do not need the control condition of pressure in the shift converter like this, be more conducive to simplify the control of processing condition.In addition, in heating before the high temperature carburizing nitrogenize and the high temperature carburizing nitridation process, by adopting aforementioned preferred furnace atmosphere pressure, the heat-up rate of workpiece is promoted rapidly, eliminate better and alleviate the unbalanced phenomenon of temperature, under higher atmosphere pressure, ammonia also is easier to be injected in the heating chamber, simultaneously, the nitrogen that penetrates into work piece surface also is difficult for escaping; But in the heat-processed before the high temperature carburizing nitrogenize, furnace atmosphere pressure generally is not less than 110Torr, otherwise nitrogen atmosphere obviously weakens failing to be convened for lack of a quorum, and brings thus intensification inefficiency, the unequal negative impact of Heating temperature (can referring to Fig. 4).
For other purpose and the consideration of processing effect, in the above-mentioned steel work piece surface nicarbing treatment process, also can adopt different furnace atmosphere pressure in the different steps of technique.For example, the temperature-fall period after the high temperature carburizing nitrogenize is finished, quenching and preserving heat stage and quench cooled stage can be adopted lower atmosphere pressure.Preferably, cooling after we can finish the high temperature carburizing nitrogenize and quenching and preserving heat process (if in the high temperature carburizing nitridation process diffusion phase is set then also can comprise diffusion phase) are set under the following vacuum state of 1Torr, can disperse like this foreign matters such as removing the oxide compound be attached on the workpiece and grease, make the surface of workpiece be in good state in complete man-hour.Further, described quenching and preserving heat and quench cooled process can make the workpiece of temperature homogeneous be quenched in quenching oil, at this moment, the ambiance pressure in quench cooled stage usually is controlled at standard atmosphere and depresses, but the quench cooled stage is preferably adopted the decompression quenching mode that is lower than standard atmospheric pressure, can change like this cooling characteristic of quenching oil, the Hardness Distribution homogeneous of capable of regulating hardened layer reduces the generation of distortion thus.Therefore in the whole process of steel work piece surface nicarbing treatment process, the ambiance pressure of different steps can be identical, also can distinguish control, and different atmosphere pressure control modes can be brought different technique effect (can referring to Fig. 4).
Above-mentioned steel work piece surface nicarbing treatment process, preferred in the heat-processed before reaching described carburizing temperature, by a whipping appts is set furnace gas is formed than strong convection, the time of this heat-processed preferably is controlled at 50min~70min.Steel workpiece of the present invention in the heating chamber of packing into after, make furnace air be replaced as nitrogen by vacuumizing first, workpiece heats in the nitrogen atmosphere environment, in the nitrogen gas generation convection current, make the atmosphere ambient windstream form more strong convection by whipping appts (for example stove internal fan), even it is more to put into like this workpiece quantity of heating chamber, also can realize rapid intensification, can also solve simultaneously because the different unbalanced problems of temperature that produce in shove charge position.
In the above-mentioned steel work piece surface nicarbing treatment process, the temperature T of described high temperature carburizing 3Can be set as comparatively high temps, so that carburizing time shortens, but preferably in 800 ℃~950 ℃ scopes, set among the present invention.Time (the t of described high temperature carburizing nitridation process 4) can be optimized according to the degree of depth of nicarbing layer, the present invention preferably is controlled at 1h~5h.When the degree of depth of desired nicarbing layer is larger, the time of high temperature carburizing nitrogenize can be set in more than the 10h.
Above-mentioned steel work piece surface nicarbing treatment process, be preferably 1min~8min the described pitch time that passes at intervals chain unsaturated hydrocarbons gas, and the amount that at every turn passes into chain unsaturated hydrocarbons gas is preferably 0.05%~0.25% of described heating chamber volume; Be 1min~8min the described pitch time that passes at intervals ammonia, and the amount that at every turn passes into ammonia is 0.05%~0.25% of described heating chamber volume.According to our repeatedly observation and experiment, if a feed rate of unsaturated hydrocarbons gas or ammonia is lower than 0.05% of heating chamber volume, perhaps the timed interval surpasses 8min, the gas volume deficiency that nicarbing is used then easily occurs, and then cause carburizing degree or the unbalanced problem of nitrogenize amount; Otherwise too short if a feed rate of unsaturated hydrocarbons gas or ammonia surpasses 0.25% or pitch time of supplying with of heating chamber volume, then the gas used of nicarbing easily produces surplus, may cause like this increase of impurity.
Above-mentioned steel work piece surface nicarbing treatment process, described chain unsaturated hydrocarbons gas can be one or more mixing in ethene, propylene, acetylene, the methylacetylene, particularly preferably be acetylene gas, because according to our experiment, its thermolysis is easier.Also can be the mixture of aforementioned gas two or three, for example adopt the mixed gas of ethene and acetylene.
In the above-mentioned steel work piece surface nicarbing treatment process, the quenching temperature of described quenching and preserving heat can be set according to the hardenability of workpiece material, and the present invention preferably is controlled at 750 ℃~900 ℃.By the quenching and preserving heat measure, can effectively eliminate the unbalanced problem of temperature of workpiece, but for the nitrogen that penetrates into workpiece is not escaped, preferably during this period still intermittent supply with ammonia.
Compared with prior art, the invention has the advantages that:
(1) treatment process of the present invention is owing to adopting intermittent type to pass into nicarbing medium mode, and in short-term carburizing amount is high, unsaturated hydrocarbon and ammonia with greater activity can be decomposed and reaction in surface and the rapid generation of workpiece by preferentially adsorbed, the impurity level that produces is less, it is general not as the limitation of the conventional thought of nicarbing medium that this has broken chain unsaturated hydrocarbons gas, and can take precautions against the unbalanced and nitrogenize unbalanced problem of carburizing;
(2) in the treatment process of the present invention, because inert atmosphere gases can realize convection current by modes such as stirring, disturbances under heating condition, workpiece is heated up rapidly, even under the condition of high-density shove charge, also can solve the workpiece unbalanced problem of being heated;
(3) treatment process of the present invention is owing to adopting intermittent to pass into the mode of carburizing medium gas and ammonia, nicarbing and diffusion hocket repeatedly, because carburizing amount and nitriding amount can reach very high level at short notice, this can prevent effectively that cementite from being separated out;
(4) in the treatment process of the present invention, because workpiece is to be heated to corresponding nicarbing temperature in nitrogen atmosphere, the vacuum oven that does not therefore need to use high-seal has reduced Meteorological and the running cost of equipment as heating installation; In addition, ammonia also can relatively easily supply in the heating chamber, penetrates into the interior nitrogen of workpiece when dropping to quenching temperature or carrying out quenching and preserving heat, and the phenomenon that nitrogen is escaped can not occur.
Generally speaking, treatment process of the present invention have equipment simple, drop into little, the advantages such as intensification efficient is high, good product quality, can be used for hardening treatment is carried out on the surface of the steel mechanical parts such as gear, wheel shaft, cam, strengthen the abrasion resistance properties of steel workpiece, improve the fatigue strength of steel workpiece, in component of machine processing treatment from now on, have important using value.
Description of drawings
Fig. 1 is the structural representation (main looking) of used treatment facility in the nicarbing treatment process of the embodiment of the invention.
Fig. 2 is the structural representation (side-looking, broken section) of used treatment facility in the nicarbing treatment process of the embodiment of the invention.
Fig. 3 is near the Hardness Distribution chart (ordinate zou represents temperature, and X-coordinate represents hardness) of the part test steel work piece surface of processing through nicarbing in the embodiment of the invention.
Fig. 4 is the process route chart (" quench and keep " i.e. among Fig. 4 be " insulation is quenched ", and " quenching " i.e. after " quench and keep " be " quench cooled ") of nicarbing treatment process of the present invention.
Marginal data:
1, nicarbing stove; 2, heating chamber; 3, cup; 4, oil groove; 5, carrying device in the stove; 6, lifting device; 7, tubular heater; 8, agitator; 9, refractory materials; 10, radiation formula tubular heater; 11, thermopair; 12, fan; 13, Vacuum door; 14, inboard Vacuum door; 15, heat-resisting door.
Embodiment
The invention will be further described with concrete preferred embodiment below in conjunction with Figure of description, but protection domain not thereby limiting the invention.
Embodiment:
A kind of steel work piece surface nicarbing treatment process of the present invention, this treatment process is used nicarbing stove 1 illustrated in figures 1 and 2, and the furnace body of nicarbing stove 1 mainly is made of heating chamber 2 and cup 3; Cup 3 is with the oil groove 4 of quenching usefulness.Also be provided with carrying device 5 in the stove that can between cup 3 and heating chamber 2, move in the cup 3, in the pallet of carrying device 5 pending steel workpiece be housed in the stove; Also be provided with in the cup 3 and after nicarbing finishes workpiece put into the lifting device 6 that oil groove 4 carries out the quenching oil immersion.In addition, in cup 3, also be provided with for the tubular heater 7 of heating oil tank 4 quenching oil of containing and the agitator 8 that is used for making the quenching oil circulation, also comprise in addition for the water cooling plant of Cooling Quenching oil and the thermopair of detection quenching oil temperature etc.
In the heating chamber 2 of the present embodiment nicarbing stove 1 3m is arranged 3Volume, be embedded in the fan 12 that heating chamber 2 inside on the refractory materials 9 are equipped with atmosphere gas (nitrogen) in the radiation formula tubular heater 10 as heating source, the thermopair 11 that detects temperature in the stove and the action of forced stirring stove, this kind structure design can make the workpiece in the stove be subjected to thermal balance and make the intensification of workpiece rapid.In addition, in heating chamber 2 and cup 3, vacuum pumping hardware is housed separately, can carries out independently the control of room pressure separately.
Nicarbing stove in the present embodiment also comprises not the in the drawings gas control equipment of expression, and it can be connected with sources of the gas such as source nitrogen, acetylene source and ammonia sources as required.
The steel work piece surface nicarbing treatment process of the present embodiment mainly may further comprise the steps (can referring to Fig. 4):
(1) prepares workpiece: at first, the Vacuum door 13 of cup 3 inlet sides is opened, send in the cup 3 after one cylindrical steel workpiece (the cylindrical experiment slice of diameter 16mm, high 30mm that the 15CrMo steel is made) being positioned over the pallet of carrying device 5 in the stove, Vacuum door 13 is closed; Start vacuum pumping hardware, behind the Bas Discharged in cup 3 and the heating chamber 2, by gas control equipment nitrogen is imported in cup 3 and the heating chamber 2, as nitrogen atmosphere pressure recovery to an a standard atmospheric pressure (P wherein 4=760Torr) after, cup 3 and heating chamber 2 have been finished by the displacement of air to nitrogen atmosphere.
(2) high temperature carburizing nitrogenize: under the state that the Vacuum door 13 of cup 3 inlet sides is closed, the inboard Vacuum door 14 of cup 3 and the heat-resisting door 15 of heating chamber 2 are opened simultaneously, the pallet that the interior carrying device 5 of startup stove will be equipped with workpiece is together released in the furnace chamber of sending into heating chamber 2, close inboard Vacuum door 14 and heat-resisting door 15, when start stirring with fan 12, give the radiation formula tubular heater 10 energising beginning heat temperature raisings of heating chamber 2, make furnace gas form convection current by fan 12 in the whole nicarbing temperature-rise period, until the temperature in the heating chamber 2 reaches 870 ℃ of (T of nicarbing temperature of steel workpiece in the present embodiment 3) time, to acetylene gas (chain unsaturated hydrocarbons) and the ammonia of heating chamber 2 interior intermittents supplies as the nicarbing medium, be 5min pitch time, passes into the acetylene gas of 6NL and the ammonia of 6NL at every turn by gas control equipment, repeatedly carry out the time t of whole high temperature carburizing nitridation process 24 times 4Be controlled at 2h; The furnace atmosphere pressure of high temperature carburizing nitridation process remains aforesaid P 4Constant (being 760Torr).
(3) quench treatment: after the high temperature carburizing nitrogenize, it is soaking time t that workpiece continues to be incubated 30min(with 870 ℃ of quenching temperatures in heating chamber 2 5=30min), in the quenching and preserving heat process still intermittent pass into ammonia, furnace atmosphere pressure all remains aforesaid P 4Constant (being 760Torr); Then open inboard Vacuum door 14 and heat-resisting door 15, the pallet that the interior carrying device 5 of startup stove will be equipped with workpiece shifts out and is back in the cup 3 from heating chamber 2, start lifting device 6, workpiece transferred to proceed the oil bath quench treatment in the oil groove 4, oil bath temperature is controlled at 60 ℃, begin to vacuumize this moment, and the ambiance pressure-controlling that makes the quench cooled stage is finished the nicarbing processing to the steel work piece surface in 200Torr quenchings of reducing pressure after quench cooled is processed.
Workpiece after processing by above-mentioned the present embodiment can observe by micro Vickers the result of the Hardness Distribution in the 0.3kg loading situation, test result as shown in Figure 3, we detect the cementation zone of the effective case depth that has formed 0.35mm.

Claims (10)

1. steel work piece surface nicarbing treatment process, may further comprise the steps: the steel workpiece is packed in the heating chamber, vacuumize first and pass into again nitrogen, the steel workpiece is in the nitrogen atmosphere, furnace atmosphere pressure is controlled at more than the 110Torr, then heating makes the steel workpiece reach the nicarbing temperature, keep pressure in the aforementioned stove, and pass at intervals unsaturated hydrocarbons gas and ammonia carries out the high temperature carburizing nitrogenize, after finishing, the high temperature carburizing nitrogenize cools to quenching temperature, then carry out quenching and preserving heat and quench cooled, finish at last the nicarbing of steel work piece surface is processed.
2. steel work piece surface nicarbing treatment process according to claim 1, it is characterized in that: described high temperature carburizing nitridation process comprises the nicarbing stage of leading portion and the diffusion phase of back segment.
3. steel work piece surface nicarbing treatment process according to claim 2 is characterized in that: in the temperature-fall period and quenching and preserving heat process after the diffusion phase of described high temperature carburizing nitrogenize, the diffusion, furnace atmosphere pressure is controlled at below the 1Torr.
4. steel work piece surface nicarbing treatment process according to claim 1 and 2 is characterized in that: in the whole process that described nicarbing is processed, furnace atmosphere pressure is controlled at 500Torr~800Torr.
5. according to claim 1 and 2 or 3 described steel work piece surface nicarbing treatment processs, it is characterized in that: described quenching and preserving heat and quench cooled process adopt quenching oil to carry out quench treatment, adopt ambiance pressure to be lower than the decompression quenching mode of standard atmospheric pressure in the quench cooled stage.
6. according to claim 1 and 2 or 3 described steel work piece surface nicarbing treatment processs, it is characterized in that: reach in the front heat-processed of described nicarbing temperature, make furnace gas form convection current by whipping appts, the time of this heat-processed is controlled at 50min~70min.
7. according to claim 1 and 2 or 3 described steel work piece surface nicarbing treatment processs, it is characterized in that: the temperature of described high temperature carburizing nitrogenize is 800 ℃~950 ℃, and the time of described high temperature carburizing nitridation process is controlled at 1h~5h.
8. according to claim 1 and 2 or 3 described steel work piece surface nicarbing treatment processs, it is characterized in that: be 1min~8min the described pitch time that passes at intervals chain unsaturated hydrocarbons gas, and the amount that at every turn passes into chain unsaturated hydrocarbons gas is 0.05%~0.25% of described heating chamber volume; Be 1min~8min the described pitch time that passes at intervals ammonia, and the amount that at every turn passes into ammonia is 0.05%~0.25% of described heating chamber volume.
9. according to claim 1 and 2 or 3 described steel work piece surface nicarbing treatment processs, it is characterized in that: described chain unsaturated hydrocarbons gas is one or more mixing in ethene, propylene, acetylene, the methylacetylene.
10. according to claim 1 and 2 or 3 described steel work piece surface nicarbing treatment processs, it is characterized in that: the quenching temperature of described quenching and preserving heat is controlled at 750 ℃~900 ℃.
CN2013103423431A 2013-08-07 2013-08-07 Surface carburization and nitridation treatment method for steel workpiece Pending CN103361594A (en)

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Publication number Priority date Publication date Assignee Title
TWI554467B (en) * 2015-11-18 2016-10-21 Metal Ind Res & Dev Ct Micro-nanometer processing device
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CN117286447B (en) * 2023-09-11 2024-04-09 苏州全项精密模具有限公司 Tooth die mould surface nitridation treatment facility

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Application publication date: 20131023