CN103981482A - Aluminum extrusion die and surface strengthening and toughening treatment process - Google Patents
Aluminum extrusion die and surface strengthening and toughening treatment process Download PDFInfo
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Abstract
The invention relates to an aluminum extrusion die and its surface strengthening and toughening treatment process. The process aims to improve surface strengthening and toughening performance of the aluminum extrusion die. By a two-stage process of doping of N before multi-element penetration of O-S-N, thicknesses of a strengthened layer and a diffusion layer in a penetration layer are both increased at different levels in comparison with an isothermal method, and it is ensured that bonding ability of the penetration layer and a matrix is better. Hardness gradient of the penetration layer is milder, penetration layer peeling time is put off, and life of the die is effectively prolonged. In addition, based on the two-stage process, thickness and strength of the diffusion layer are both raised effectively by the use of a Ce/La rare earth compound for catalysis and by the use of an NH4Cl powder for cleaning and penetration treatments; and an antifriction complex phase layer containing Fel-xS and Fe3O4 phases and a strengthened layer containing Fe2-3N, gamma'-Fe4N and other high hardness and toughness phases can be obtained. Thus, the penetration layer satisfies ideal wearing layer conditions of tribological requirements.
Description
Technical field
The present invention relates to technical field of mold, is a kind of the Aluminum-Extruding Die and surface toughening treatment process thereof specifically.
Background technology
Correlative study both at home and abroad shows, it is to improve its use properties that the Aluminum-Extruding Die is adopted to surface toughening treatment process, one of effective means increases the service life, adopt traditional gas nitriding treatment process, not only its nitrogenation treatment technology cycle is long, and nitride layer matter is crisp, in extrusion process, easily peel off and cause aluminium alloy section surface to scratch, the defects such as wall thickness dimension is overproof, for this reason, physical vapor deposition (PVD coating) method is successively developed in correlative study both at home and abroad, ion nitriding, polybasic ion composite algorithm, the surface toughening New Process for Treatment such as O-S-N multiple permeation soft nitriding.
China's the Aluminum-Extruding Die surface toughening treatment technology is also relatively backward at present, still has larger gap compared with Foreign Advanced Lerel.Because China's aluminium section bar in recent years obtains at building field on the basis of widespread use, constantly expand promoting the use of at industrial circle, and commercial aluminum alloy section material section specification is large, complex structure etc., the Aluminum-Extruding Die surface toughening performance has been proposed to requirements at the higher level, suddenly treat further to improve the Aluminum-Extruding Die surface toughening treatment process state of the art, therefore, the technical study of this aspect has caused the attention of relevant industry, is increasing input and is carrying out the technical study of the Aluminum-Extruding Die strength-toughening treatment process.
Comparative analysis the gas nitriding of current domestic and international application, wet nitriding and ammonia introducing dropleting alcohol gas soft nitriding treatment process achievement in research find, above-mentioned technique all exists that infiltration layer is crisp and loose in various degree, Hardness Distribution gradient is steep and with the deficiency of the aspect such as matrix bonding properties is poor, wherein ion Plasma Nitriding Treatment can solve the relative contradiction of surface hardness and toughness, but is difficult to prove effective for type hole more complicated and narrow punch die; Physical vapor deposition (PVD coating) method and chemical vapour deposition (CVD coating) are owned by France in high-temperature processing technology, its treatment temp is all greater than 750 DEG C, and the Aluminum-Extruding Die tempering temperature is conventionally 580 DEG C of left and right, the core structure and the performance that adopt PVD method or CVD method meeting havoc the Aluminum-Extruding Die, be not suitable for using as the Aluminum-Extruding Die surface toughening treatment process.Therefore, research adopts the multiple permeation treatment process such as O-S-N, S-C-N, S-N-B, has become the main direction of studying of relevant industry raising the Aluminum-Extruding Die surface toughening performance both at home and abroad.But it is inadequate that existing multiple permeation treatment process exists thickness and the solution strengthening of diffusion layer more, and be prone to the microstructure defects such as veiny crystalline substance, the co-penetration layer hardness gradient problem such as steep that distributes, make it ooze altogether strengthening layer and easily peel off in extrusion process of production, cause that extrusion mould is scrapped etc.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, technical problem to be solved by this invention is to provide a kind of the Aluminum-Extruding Die surface toughening treatment process that can significantly improve the Aluminum-Extruding Die surface toughening performance, and and then provides a kind of surface toughening performance good the Aluminum-Extruding Die.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of the Aluminum-Extruding Die surface toughening treatment process, comprises the following steps:
Step 1, pending the Aluminum-Extruding Die is placed under 530～560 DEG C of heating and thermal insulation conditions, logical ammonia is processed 3～4 hours, and ammonia flow is 0.10～0.30m
3/ h, ammonia dissociation rate is controlled at 22～30%, adopts metallic surface cleaning activation agent to process the Aluminum-Extruding Die work belt surface in treating processes;
Step 2, the Aluminum-Extruding Die that step 1 is obtained continue to be placed under 560～590 DEG C of heating and thermal insulation conditions, and logical ammonia and instillation mixed solution are processed 3～4 hours, and ammonia flow is 0.10～0.30m
3/ h, ammonia dissociation rate is controlled at 28～36%, described mixed solution is mixed by thiocarbamide, the Ce/La rare earth compound of 8～15 weight parts and the dehydrated alcohol of 500 parts by volume of 10～18 weight parts, described weight part: parts by volume=g: ml, adopts metallic surface cleaning activation agent to process the Aluminum-Extruding Die work belt surface in treating processes;
Wherein, the cleaning activation agent of described metallic surface is by the NH of 0.8～1.3 parts by volume
4the quartz sand of Cl and 6 parts by volume mixes.
The Aluminum-Extruding Die of the present invention, after above-mentioned surface toughening is processed, its work belt surface has co-penetration layer, and described co-penetration layer comprises antifriction complex phase layer, strengthening layer and diffusion layer from outside to inside successively, and described antifriction complex phase layer contains Fe
1-xs and Fe
3o
4phase, described strengthening layer contains Fe
2-3n and γ '-Fe
4n phase, the thickness of described strengthening layer is 10～13 μ m, and described diffusion layer is the solution strengthening district of nitrogen in α-Fe, and the thickness of described diffusion layer is 150～180 μ m.
The present invention compared with prior art, has following beneficial effect:
1, adopt the two-stage method technique of " first oozing N, rear O-S-N multiple permeation ", make strengthening layer (bright layer), thickness of diffusion layer in its co-penetration layer obtaining all have increase in various degree than isothermal method, the bonding properties of guaranteeing co-penetration layer and matrix is better, thereby obtain comparatively desirable alloying layer thickness and microhardness, the co-penetration layer hardness gradient obtaining is milder than isothermal method, postpone infiltration layer and peeled off the time, thereby effectively improved die life;
2,, on the basis of two-stage method technique, the present invention adopts Ce/La rare earth compound to urge to ooze and NH
4cl powder carries out cleaning and oozes altogether processing, has improved the nitrogen concentration in diffusion layer, and the thickness of diffusion layer and intensity are all effectively promoted, and can obtain containing Fe simultaneously
1-xs, Fe
3o
4the antifriction complex phase layer of phase, and contain Fe
2- 3n, γ '-Fe
4the strengthening layer (bright layer) of the high rigidity such as N, obdurability phase, makes the co-penetration layer that the present invention obtains can meet preferably the desirable wearing layer condition that tribology requires.
Brief description of the drawings
Figure 1 shows that the process schematic representation of the embodiment of the present invention.
Figure 2 shows that the co-penetration layer metallographic microstructure figure of the embodiment of the present invention.
Figure 3 shows that the X ray diffracting spectrum of the co-penetration layer of the embodiment of the present invention.
Figure 4 shows that the co-penetration layer microhardness distribution curve of the embodiment of the present invention.
Figure 5 shows that section model is the mould sectional schematic diagram of Y5329.
Figure 6 shows that section model is the mould sectional schematic diagram of Y5336.
Figure 7 shows that section model is the mould sectional schematic diagram of L8601.
Figure 8 shows that section model is the mould sectional schematic diagram of L8603.
Figure 9 shows that section model is the mould sectional schematic diagram of L8607.
Figure 10 shows that section model is the mould sectional schematic diagram of YS5054.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, below in conjunction with embodiment and coordinate accompanying drawing to be explained in detail.
The design of most critical of the present invention is: adopt the two-stage method technique of " first oozing N, rear O-S-N multiple permeation ", and on the basis of two-stage method technique, adopt Ce/La rare earth compound to urge and ooze and NH
4cl powder carries out cleaning and oozes altogether processing.
Concrete, the Aluminum-Extruding Die surface toughening treatment process of the present invention, comprises the following steps:
Step 1, pending the Aluminum-Extruding Die is placed under 530～560 DEG C of heating and thermal insulation conditions, logical ammonia is processed 3～4 hours, and ammonia flow is 0.10～0.30m
3/ h, ammonia dissociation rate is controlled at 22～30%, adopts metallic surface cleaning activation agent to process the Aluminum-Extruding Die work belt surface in treating processes;
Step 2, the Aluminum-Extruding Die that step 1 is obtained continue to be placed under 560～590 DEG C of heating and thermal insulation conditions, and logical ammonia and instillation mixed solution are processed 3～4 hours, and ammonia flow is 0.10～0.30m
3/ h, ammonia dissociation rate is controlled at 28～36%, described mixed solution is mixed by thiocarbamide, the Ce/La rare earth compound of 8～15 weight parts and the dehydrated alcohol of 500 parts by volume of 10～18 weight parts, described weight part: parts by volume=g: ml, adopts metallic surface cleaning activation agent to process the Aluminum-Extruding Die work belt surface in treating processes;
Wherein, the cleaning activation agent of described metallic surface is by the NH of 0.8～1.3 parts by volume
4the quartz sand of Cl and 6 parts by volume mixes.
Know-why of the present invention is as follows:
1, only ooze N (being step 1) early stage, to increase the concentration gradient of die working length surfactivity nitrogen-atoms, strengthening nitrogen-atoms constantly by surface to inner diffusion, thereby can increase thickness and the intensity of diffusion layer; Later stage is carried out O-S-N multiple permeation (being step 2) again, to obtain top layer as Fe
1-xs, Fe
3o
4lubricated thin layer, can be used as antifriction complex phase layer, effectively stop " interlock " between aluminum metal and mold work belt surface, reduce the frictional force of die working length, reduce its frictional wear, avoid or reduce its infiltration layer peeling off; Inferior top layer is fine and close Fe
2-3n, Fe
4n (γ ' phase) nitride, has the hardened layer (bright layer) that obdurability has both, and has the diffusion layer of Rational Thickness, guarantees that the bonding properties of co-penetration layer and matrix is better, thereby obtains comparatively desirable alloying layer thickness and microhardness.
2, adopt by NH
4the metallic surface cleaning activation agent that Cl and quartz sand are mixed, make mold work belt surface in follow-up heat-processed, can remove the passive film of die surface, make workpiece surface sensitization and purifying, promote the diffusion of nitrogen-atoms to infiltrate, improve the nitrogen concentration in diffusion layer, namely dissolved more nitrogen-atoms its microstress is significantly increased, made to obtain effectively and promote as the diffusion layer intensity of transition layer.
3, adopt Ce/La catalysis of rare-earth compound multiple permeation treatment process, the one, active very strong rare earth atom is by activation workpiece surface and adsorption, weaken the molecule bonding force of diffusion medium, can accelerate penetration enhancer decomposes, the 2nd, the infiltration of large-sized rare earth atom, make iron atom lattice distortion around, produce room, the defects such as dislocation, thereby form diffusion " passage ", increase its spread coefficient, promote other to ooze altogether the infiltration diffusion of atom to matrix inside, further improve the intensity of infiltration layer, hardness and wear resistance, also make nitrided layer hardness gradient more tend towards stability, the desirable friction layer hardness gradient that As soon as possible Promising Policy tribology requires distributes.
From foregoing description, beneficial effect of the present invention is: improved the bonding properties of co-penetration layer and matrix, made co-penetration layer thickness and microhardness even more ideal, co-penetration layer hardness gradient distributes more mild, co-penetration layer is incrust, and die life improves greatly.
Further, in step 1, described the Aluminum-Extruding Die is first through cleaning, dry, preheating logical ammonia processing again after 1～2 hour at 530～560 DEG C.
Further, in step 2, the rate of addition of described mixed solution is 20～60d/min.
Further, described step 1 and step 2 are carried out in well formula heat treatment furnace, and described the Aluminum-Extruding Die is placed in mould and oozes altogether in thermal treatment special frame, and the bottom storing that described mould oozes thermal treatment special frame altogether has the cleaning activation agent of described metallic surface.
Further, after step 2 has been reacted, adopt the logical cold mode of nitrogen furnace to carry out cooling to the Aluminum-Extruding Die.
Embodiment
With aluminium section bar hot extrude mould H
13steel (4Cr
5moSiV
1) be example, please refer to shown in Fig. 1, the Aluminum-Extruding Die surface toughening treatment process of the present embodiment is as follows:
(1) after pending the Aluminum-Extruding Die is cleaned up, dried, interval is placed in mould and oozes altogether in thermal treatment special frame, and the metallic surface cleaning activation agent of putting specified amount at its frame bottom is (by NH
4cl evenly mixes with the ratio that quartz sand is 0.8～1.3: 6 according to volume ratio), make mold work belt surface in follow-up heat-processed, can remove 4Cr
5moSiV
1the passive film Cr on steel extrusion mould surface
2o
3, cleaning activation die surface, is beneficial to N, S, O atom is absorbed and infiltrates by its top layer.
(2) heat to first stage technological temperature T at well formula heat treatment furnace
1when (530～560 DEG C), the above-mentioned special frame of getting mould ready is hung onto in stove, carry out as shown in Figure 1 the logical ammonia nitriding of first stage and process t
1(3～4 hours) time, monitor its ammonia flow between 0.10～0.30m with suspended body flowmeter
3/ h, monitor its ammonia dissociation rate between 22～30% with glass resolution ratio measuring meter, to improve the nitrogen atom content of die surface layer, increase the solid solution strengthening effect of its thickness of diffusion layer and nitrogen thereof, make to have between the strengthening layer of follow-up formation and matrix the transition layer of Rational Thickness, can build milder hardness gradient and distribute.
(3) in the time that the logical ammonia nitriding of first stage is finished dealing with, well formula heat treatment furnace is heated to subordinate phase technological temperature T
2(560～590 DEG C), N, the S, the O that carry out subordinate phase ooze processing altogether, and the treatment time is t
2(3～4 hours).In treating processes, adopt the mode that passes into ammonia and drip mixed solution, monitoring ammonia flow with suspended body flowmeter is 0.10～0.30m
3/ h, between 28～36%, dissolves in 10～18g thiocarbamide, 8～15gCe/La rare earth compound preparation mixed solution according to the dehydrated alcohol of 500ml with glass resolution ratio measuring meter monitoring ammonia dissociation rate, with the rate of addition of threeway dropper control mixed solution be 20～60d/min.
(4) ooze altogether while finishing dealing with when subordinate phase, adopt the cold mode of logical nitrogen furnace by mold cools down to room temperature.
Detect and analyze:
One, metallographic microstructure analysis and X-ray diffraction analysis
The Aluminum-Extruding Die that above-described embodiment is obtained adopts metaloscope to observe its co-penetration layer tissue, and the metallographic microstructure of acquisition as shown in Figure 2; The Aluminum-Extruding Die that above-described embodiment is obtained adopts X-ray diffractometer to analyze the phase structure composition of its co-penetration layer microstructure, and the X ray diffracting spectrum of acquisition as shown in Figure 3.
In Fig. 3,1. represent Fe
2-3n, 2. represents Fe
4n (γ ' phase), 3. represents Fe
3o
4, 4. represent α-Fe, 5. represent Fe
1-xs.
Shown in Fig. 2 and Fig. 3, the co-penetration layer that the present invention obtains, comprises three layers from outside to inside.Wherein outermost layer is antifriction complex phase layer, in antifriction complex phase layer, contains Fe
1-xs, Fe
3o
4phase, and the infiltration layer of isothermal method only has Fe
2o
3phase, the Fe softer than matrix matter
1-xs, Fe
3o
4rete can lubricate, effectively stops " interlock " between aluminum metal and mold work belt surface, reduces the frictional force of die working length, reduces its frictional wear, avoids or reduce its infiltration layer peeling off; Middle bright layer is strengthening layer, and the thickness of strengthening layer is 10～13 μ m, contains fine and close Fe in strengthening layer
2-3n, Fe
4n (γ ' phase) nitride, therefore obdurability has both, and the strengthening layer thickness that isothermal method obtains is only 2～7 μ m; Innermost layer is diffusion layer near the region of bright layer corrosion-vulnerable, is the solution strengthening district of nitrogen in α-Fe, and the thickness of described diffusion layer is 150～180 μ m, and the thickness of diffusion layer that isothermal method obtains is only 120～150 μ m.
From above-mentioned analysis, in the co-penetration layer that the present invention obtains, not only possesses the antifriction complex phase layer of lubricate, and strengthening layer (bright layer), thickness of diffusion layer have all had increase in various degree than isothermal method, the bonding properties of guaranteeing co-penetration layer and matrix is better, thereby obtain comparatively desirable alloying layer thickness and microhardness, postpone infiltration layer and peel off the time, effectively improve die life.
Two, co-penetration layer microhardness distribution detects
The Aluminum-Extruding Die that above-described embodiment is obtained adopts microhardness tester to detect the vickers hardness number of its co-penetration layer different sites, draws its hardness gradient distribution curve as shown in Figure 4.
Known as shown in Figure 4, the co-penetration layer hardness gradient that the present invention obtains distributes and tends towards stability, and can meet the desirable friction layer hardness gradient distribution that tribology requires, and meets the service requirements of the Aluminum-Extruding Die in high temperature, high pressure, high friction, postpone infiltration layer and peel off the time, effectively improve die life.
Three, aluminium alloy extruded throughput detects
Adopt the mould of different section model to carry out surface toughening processing according to the technique described in above-described embodiment, follow the tracks of and investigate its aluminium alloy extruded throughput, result is as shown in table 1 below.
Table 1, the mould amount of being pressed through cartogram (unit: ton)
Wherein, the mould section of section model Y5329 as shown in Figure 5, the mould section of section model Y5336 as shown in Figure 6, the mould section of section model L8601 as shown in Figure 7, the mould section of section model L8603 as shown in Figure 8, as shown in Figure 9, the mould section of section model YS5054 as shown in figure 10 for the mould section of section model L8607.
From shown in table 1, the co-penetration layer that the present invention obtains, can meet the service requirements of the Aluminum-Extruding Die in high temperature, high pressure, high friction, effectively improves die life.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention and accompanying drawing content to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. a Aluminum-Extruding Die surface toughening treatment process, is characterized in that, comprises the following steps:
Step 1, pending the Aluminum-Extruding Die is placed under 530～560 DEG C of heating and thermal insulation conditions, logical ammonia is processed 3～4 hours, and ammonia flow is 0.10～0.30m
3/ h, ammonia dissociation rate is controlled at 22～30%, adopts metallic surface cleaning activation agent to process the Aluminum-Extruding Die work belt surface in treating processes;
Step 2, the Aluminum-Extruding Die that step 1 is obtained continue to be placed under 560～590 DEG C of heating and thermal insulation conditions, and logical ammonia and instillation mixed solution are processed 3～4 hours, and ammonia flow is 0.10～0.30m
3/ h, ammonia dissociation rate is controlled at 28～36%, described mixed solution is mixed by thiocarbamide, the Ce/La rare earth compound of 8～15 weight parts and the dehydrated alcohol of 500 parts by volume of 10～18 weight parts, described weight part: parts by volume=g: ml, adopts metallic surface cleaning activation agent to process the Aluminum-Extruding Die work belt surface in treating processes;
Wherein, the cleaning activation agent of described metallic surface is by the NH of 0.8～1.3 parts by volume
4the quartz sand of Cl and 6 parts by volume mixes.
2. the Aluminum-Extruding Die surface toughening treatment process according to claim 1, is characterized in that: in step 1, described the Aluminum-Extruding Die is first through cleaning, dry, preheating logical ammonia processing again after 1～2 hour at 530～560 DEG C.
3. the Aluminum-Extruding Die surface toughening treatment process according to claim 1, is characterized in that: in step 2, the rate of addition of described mixed solution is 20～60d/min.
4. the Aluminum-Extruding Die surface toughening treatment process according to claim 1, it is characterized in that: described step 1 and step 2 are carried out in well formula heat treatment furnace, described the Aluminum-Extruding Die is placed in mould and oozes altogether in thermal treatment special frame, and the bottom storing that described mould oozes thermal treatment special frame altogether has the cleaning activation agent of described metallic surface.
5. the Aluminum-Extruding Die surface toughening treatment process according to claim 4, is characterized in that: after step 2 has been reacted, adopt the logical cold mode of nitrogen furnace to carry out cooling to the Aluminum-Extruding Die.
6. a Aluminum-Extruding Die, is characterized in that: the work belt surface of described the Aluminum-Extruding Die is provided with co-penetration layer, and described co-penetration layer comprises antifriction complex phase layer, strengthening layer and diffusion layer from outside to inside successively, and described antifriction complex phase layer contains Fe
1-xs and Fe
3o
4phase, described strengthening layer contains Fe
2-3n and γ '-Fe
4n phase, the thickness of described strengthening layer is 10～13 μ m, and described diffusion layer is the solution strengthening district of nitrogen in α-Fe, and the thickness of described diffusion layer is 150～180 μ m.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987793A (en) * | 2017-06-01 | 2017-07-28 | 广东华昌铝厂有限公司 | H13 steel molds nitrogenation treatment technology again |
| CN109183020A (en) * | 2018-08-27 | 2019-01-11 | 合肥工业大学 | A kind of preparation method of aluminum alloy surface complex gradient modified layer |
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| CN109183020A (en) * | 2018-08-27 | 2019-01-11 | 合肥工业大学 | A kind of preparation method of aluminum alloy surface complex gradient modified layer |
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| CN103981482B (en) | 2016-08-24 |
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Address after: 353000 Nanping Industrial Road, Fujian, No. 65 Applicant after: FUJIAN NANPING ALUMINIUM CO., LTD. Address before: 353000 Nanping Industrial Road, Fujian, No. 65 Applicant before: Fujian Nanping Aluminum Co., Ltd. |
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