CN1055013A - The extruding tool and mould and the manufacture method thereof of band coating - Google Patents

Abstract

The present invention proposes the tool and mould and the manufacturing process thereof of the band coating that a kind of suitable hot extrusion tubing uses, the tool and mould of design is by base material, the middle layer of vapour deposition and the wear-resistant coating on the middle layer are formed on the base material, and the middle layer is the titanium nitride layer of high nitrogen, and thickness is the 0-1 micron.Adopt physical gas-phase deposition on base material, to deposit respectively.Can obtain hardness height, coating that bonding force is good by the control deposition process parameters, the aluminium tube extrusion production proves, uses this tool and mould can significantly improve the tubing yield rate, alleviates labor strength, improves working conditions and product surface quality, prolongation tool and mould work-ing life.

Description

The extruding tool and mould and the manufacture method thereof of band coating

The present invention relates to push processing method, especially with the tool and mould of tubing extruding usefulness and to carry out the technology of surface physics vapour deposition on the base material of tool and mould in extruding relevant with tool and mould and top coat thereof.

Present most of non-ferrous metal tubing and engineering plastics tubing are hot extrusion processing. the tool and mould of hot extrusion processing usefulness will bear high temperature and powerful friction simultaneously, as push pin when hot extrusion, powerful friction will take place with the high temperature blank in whole surface, extruding pin serious wear, in use for some time, be difficult for guaranteeing tolerance of dimension; Simultaneously, the extruding wire surface bonds pressing material easily and forms the material knurl, and inner wall surface easily is scratched and causes waste product, consequent scrap rate to account for the 5-8% of total input amount when tubing is out of shape; For alleviating inner surface scratch wound, material of every extruding just needs artificial frosted extruding wire surface and smears lubricant, production efficiency is low. therefore carrying out a series of research aspect the wear-resisting and anti-stick property that improves the extruding wire surface. and the physical vapor deposition (PVD) coating technology obtained developing especially rapidly over past ten years, bearing frictional force part such as speedy steel cutting-tool, inserted tool and other form cutter and such as being used widely on the decorations such as watchcase. decorations such as watchcase generally use stainless material, its working conditions requires not harsh to the wear resistance and corrosion resistance on surface, therefore use general depositing operation can obtain meeting the coating of service requirements. this coating is often because its hardness and not enough with the bonding force of base material, be not suitable for the hot extrusion tool and mould. then should make the knife edge part of small area wear-resisting for cutter, its working conditions wants complicated than watchcase, therefore for the hardness that improves coating and the bonding force between coating and the base material, to improve the deposition process parameters of coating on the one hand, then before deposition procedures, increase on the other hand and give deposition procedures together, what mention in deposition one deck middle layer .US 4461799 documents between base material and coating is exactly to deposit the discontinuous pure metallic titanium of one deck earlier as the middle layer on the surface of body material, and then deposition one deck titanium nitride coating. the tool surface that has then selects for use pure metallic nickel or Ti-Ni alloy as the middle layer. also develop the compound coating of heterogeneous multi-layer in the last few years. but because the hot extrusion tool and mould uses 3Cr 2W 8V.4Cr5MoVlSi.W18Cr4V and some high Cr usually, Mo, W, the Mn steel alloy is made. and its working conditions is also different, and therefore above-mentioned these schemes are not suitable for the hot extrusion tool and mould yet.

The objective of the invention is to design the tool and mould and the manufacturing process thereof of the band coating that a kind of suitable hot extrusion tubing uses.

The tool and mould that the hot extrusion of the present invention design is used comprises base material and at the wear-resistant coating of substrate surface. and the component of wear-resistant coating be to meet stoichiometric titanium nitride compound substantially. and base material is a kind of in various hot extrusion tool and moulds usefulness steel and the rapid steel.

In order to improve the bonding force between coating and the base material, make the coating of tool and mould incrust in hot extrusion process, between base material and wear-resistant coating, also have one deck middle layer, the middle layer is the titanium nitride of high nitrogen.

The coating process that the present invention proposes is a physical vapor deposition TiN technology, comprise that workpiece surface gives processing, deposition procedures. desirable in the surface hardness height, the coating that matrix/coating is combined and the condition of surface of workpiece and deposition process parameters are closely related. must give processing to workpiece as the surface earlier before the deposition, this operation comprises removes Superficial Foreign Body and surface active two portions, remove Superficial Foreign Body and be meant the surperficial grease of removal, oxide compound and other pollution layer, can adopt chemical physics to clean, matting can adopt commercially available clean-out system such as shampoo and various metal cleaner, physics cleans the ultrasonic cleaning method that can adopt frequent use. and the workpiece after the cleaning is packed into after general drying in the PVD coating device, heat de-airing and the surface activation process in argon atmospher under vacuum. surface activation process is carried out under the negative bias of 500-1500V, argon gas bombards the effect that workpiece surface reaches activating surface after ionization, about 10-20 of treatment time minute, to decide on the workpiece particular case. the workpiece after processing is given on the surface can carry out surface deposition. and workpiece temperature is between 350-590 ℃ during deposition, bias voltage is 0～-240 volt, the gas total pressure remain on 0.07-1.2Pa wherein the partial pressure of working gas argon remain on 0.03-0.6Pa, the partial pressure of reactant gases nitrogen is at 0.03-0.6Pa, titanium tetrachloride vapor and nitrogen reaction with this understanding, sedimentation velocity with per second 5-80 dust is roughly stoichiometric titanium nitride coating in the generation of base material outside surface, the control depositing time just can obtain the coating of different thickness, generally between 10-50 minute. for the tone that makes coating more beautiful, more be hardness golden yellow and the outer top coat of raising, after deposition procedures, also can increase the back deposition procedures, the main partial pressure of reactant gases nitrogen of suitably adjusting is to 0.05-0.5Pa in this operation, approximately after 1-3 minute, can stop deposition, come out of the stove after the cooling.

In order between base material and wear-resistant coating, to obtain the titanium nitride middle layer of high nitrogen-containing, after substrate surface gives processing, should give deposition earlier.

Give deposition procedures and be the additional process of matrix/coating interface of obtaining, and good interface is to obtain required composition, phase structure, hardness and matrix and be coated with the important prerequisite that interlayer has the coating of enough bonding forces. when giving deposition, workpiece should remain between 350-590 ℃, bias voltage is 0～-240 volt, the gas total pressure remains in the 0.1-1.6Pa scope, wherein the partial pressure of working gas argon gas remains on 0.04-0.8Pa, the partial pressure of reactant gases nitrogen is in the 0.04-1.0Pa scope, the partial pressure of nitrogen should be higher than the partial pressure of argon, nitrogen partial pressure is strong/and the strong β of partial pressure of ar gas is in the 1-7 scope. and be in the metal titanium evaporation back and nitrogen reaction of molten state with this understanding, generated the titanium nitride inter coat of high nitrogen-containing with the sedimentation velocity of per second 5-80 dust at workpiece surface. reach required film thickness through 2-10 minute approximately and enter deposition procedures.

For making workpiece that uniform coat-thickness radially and vertically arranged, from the workpiece surface activation treatment until whole deposition process, work all is in during translation and planet rotate. and reach this purpose, workpiece can be installed in application number that the same applicant of the application's case proposes and be 90200967.2 physical vapor deposition with in the shaft-like matrix clamping device.

To give sedimentary middle layer and have the composition of design and phase structure and post-depositional top coat and have the composition and the phase structure of design in order to make, before beginning to give deposition and after the deposition end, cover operation in addition, covering on the maneuvering device is blocked base material, prevents that undesirable reactive evaporation thing is deposited on workpiece surface.

The coating process that uses the present invention to propose can obtain certain thickness titanium nitride coating on the tool and mould surface of hot extrusion, thereby these tool and mould surface hardnesses are further improved, Hv can reach 35GPa and improve 5-6 doubly, the abrasive wear life-span improves more than 150 times with comparing of coating not, matrix and be coated with interlayer and have stronger bonding force .Lc to reach more than the 50N. with the extruding pin is example, long-term big production examination shows, the surface hardness height of band coating extruding pin, incrust, matrix metal is few, can significantly improve the squeezing prod surface quality, improve more than the tubing yield rate 4-20%; Reduce under operator's high temperature matte surface and be coated with operation such as lubricant, improve working conditions. there is the extruding pin in middle layer that surface abrasion in use takes place hardly between base material and wear-resistant coating, significant prolongation tool and mould work-ing life.

Fig. 1 gives the influence curve of the gas total pressure in when deposition to bonding force, and wherein ordinate is bonding force (N), and abscissa is gas total pressure (Pa).

Fig. 2 gives the partial pressure in when deposition by force to the influence curve of bonding force, and wherein ordinate is bonding force (N), and abscissa is β.

Fig. 3 is the influence of base material temperature to bonding force, and wherein ordinate is bonding force (N), abscissa be base material temperature (℃).

Fig. 4 is the influence of negative bias to bonding force, and wherein ordinate is bonding force (N), and abscissa is negative bias (volt).

The relation curve of gas total pressure and coating microhardness when Fig. 5 is deposition, wherein ordinate is hardness (GPa), abscissa is gas total pressure (Pa).

Fig. 6 is the relation curve of the strong and coating microhardness of when deposition partial pressure, and wherein ordinate is hardness (GPa), and abscissa is β.

Fig. 7 is the relation curve of base material temperature and coating microhardness, and wherein ordinate is hardness (GPa), abscissa be base material temperature (℃).

The relation curve of negative bias and coating microhardness when Fig. 8 is deposition, wherein ordinate is hardness (GPa), abscissa is negative bias (volt).

Gas total pressure and the relation curve of friction durability when Fig. 9 is deposition, wherein ordinate is friction durability (second), abscissa is gas total pressure (Pa).

Figure 10 is when deposition partial pressure relation curve of strong and friction durability, and wherein ordinate is friction durability (second), and abscissa is β.

Figure 11 is when deposition base material temperature and the relation curve of friction durability, and wherein ordinate is friction durability (second), abscissa be base material temperature (℃).

Negative bias and the relation curve of friction durability when Figure 12 is deposition, wherein ordinate is friction durability (second), abscissa is negative bias (volt).

A is base material with 3Cr2W8v among Fig. 1-Figure 12, and b is base material with 4Cr5MoVlSi.

Figure 13 is the wear curve of various condition samples, and wherein ordinate is abrasion loss (milligram); Abscissa is wearing-in period (branch). the upper right corner is a partial enlarged drawing among the figure, and I is for no coating tool and mould, and II be that to be with TiN coating, III among the embodiment four be to be with middle layer and coating among the embodiment five.

Figure 14 is the tensile strength after depositing TiN coating on the different substrate materials and the relation curve of coat-thickness, wherein a is base material with 3Cr2W8v, b is base material with 4Cr5MoVlSi, c is to be base material with 3Cr2W8V that via nitride is handled, d is to be base material with 4Cr5MoVlSi that via nitride is handled. ordinate is tensile strength (MPa), and abscissa is coat-thickness (micron).

Figure 15 is the unit elongation after depositing TiN coating on the different substrate materials and the relation curve of coat-thickness, wherein a is base material with 3Cr2W8v, b is base material with 4Cr5MoVlSi, d is to be base material with 4Cr5MoVlSi that via nitride is handled. ordinate is unit elongation (%), and abscissa is coat-thickness (micron).

Figure 16 is the reduction of area after depositing TiN coating on the different substrate materials and the relation curve of coat-thickness, wherein a is base material with 3Cr2W8v, b is base material with 4Cr5MoVlSi, d is to be base material with 4Cr5MoVlSi that via nitride is handled. ordinate is reduction of area (%), and abscissa is coat-thickness (micron).

Figure 17 is in the tensile strength under differing temps after the depositing TiN coating on the different substrate materials. wherein ordinate is tensile strength (MPa), abscissa be temperature (℃).

Figure 18 is at the unit elongation under differing temps after the depositing TiN coating on the different substrate materials. wherein ordinate is unit elongation (%), abscissa be temperature (℃).

Figure 19 is at the reduction of area under differing temps after the depositing TiN coating on the different substrate materials. wherein ordinate is reduction of area (%), abscissa be temperature (℃).

A is base material with 3Cr2W8v among Figure 17-19, and b is base material with 4Cr5MoVlSi, c is to be base material with the 3Cr2W8V that via nitride is handled, and d is to be base material with 4Cr5MoVlSi that via nitride is handled.

The device that Figure 20 rotates for the translation simultaneously used in the physical gas-phase deposition and planet.

Further specify embodiments of the present invention and effect thereof with following indefiniteness embodiment.

One, extruding wire surface at 3Cr2W8V and 4Cr5MoVlSi steel deposits one deck pure metallic titanium middle layer earlier, and then depositing TiN coating. the depositing operation of titanium layer is that ar pressure is respectively 0.12,0.135,0.265Pa, the titanium deposition layer thickness is 0.014 micron. and then have the extruding wire surface depositing titanium nitride coating in these titanium middle layers respectively, its depositing operation is respectively gas total pressure 0.07,0.14,0.35,0.65,0.9 and 1.2Pa, partial pressure of ar gas is strong by 0.035,0.07,0.20,0.3,0.5 and 0.6Pa, nitrogen partial pressure is strong by 0.035,0.07,0.15,0.35,0.4 and 0.6Pa, 500 ℃ of base material temperatures, the deposition different time obtains 3,5,7,10 microns titanium nitride coating. measure its microhardness value in the 11-20GPa scope, bonding force is in the 30-35N scope, only 3-4 minute wearing test life-span. coating is peeled off in a large number during owing to extruding, therefore is not suitable for hot extrusion tubing. and concrete processing parameter sees Table 1.

Two, adopt example one essentially identical extruding needle construction, difference is that the middle layer is a pure metallic nickel. the depositing operation of nickel dam is that ar pressure is (1-1.6) Pa, the deposition bed thickness is 0.014 micron. and then by general TiN coating process, be that the gas total pressure is 0.15-0.65Pa, the strong 0.07-0.35Pa of partial pressure of ar gas, nitrogen partial pressure is by force 0.07-0.35Pa, 500 ℃ of deposit obtain coat-thickness and are respectively the extruding pin that the 8-10 micron does not wait. and concrete processing parameter sees Table 2. its bonding forces all less than 30N, and test shows that this extruding pin is not suitable for hot extrusion tubing yet.

Three, adopt example one essentially identical extruding needle construction, difference is that the middle layer is the Ti-Ni alloy layer. intermediate layer thickness is 0.1 micron, the partial pressure of argon gas is the 4-8 micron with the thickness of the routine process deposits TiN coating .TiN coating of table 3 by 0.135Pa. on have titanium-nickel alloy layer again during deposition, the extruding pin that has even deposit to 30 microns. measure its microhardness value in the 12-25GPa scope, no matter bonding force Lc uses the coating of the sort of process deposits less than 30N., the extruding pin that has titanium-nickel middle layer all is not suitable for extruded aluminum, exposes steel substrate once using.

Four, the TiN coating depositing operation that proposes with the present invention, obtaining the hot extrude pressing formed by base material and titanium nitride coating. concrete mode of deposition sees Table 4, coat-thickness is the 3-5 micron. measuring its surface microhardness value is 9-26GPa, bonding force Lc is 25-45N, abrasive grain wear test life-span difference is also bigger, 6, No. 7 samples can reach more than 8 minutes, did not wait in other 1-6 minute.

Compare with uncoated in the wear-out life scope of coating, the surface adhesion metal is few, and product surface quality is good, thereby has reduced non-productive operation, but coating is easily peeled off or worn and torn.

Adopt deposition process parameters preferably, be that the gas total pressure is 0.22Pa, partial pressure of ar gas is by force that the 0.12Pa. nitrogen partial pressure is 0.1Pa by force, base material temperature is 500 ℃, bias voltage is 4 microns an extruding pin for-30 volts depositing operation obtains the TiN coat-thickness, measure its surface microhardness up to 25GPa, bonding force reaches 45N, 8 minutes abrasive grain wear test life-spans. with this extruding pin extruding LF, LY, L, 5056, Ly11, it is saturating that the localized delamination or the mill of coating appears in (the tubing specification is φ (10-30) * 1 a millimeter thin-walled tube) during 5083 tubing such as aluminum or aluminum alloy such as grade when 1000 kilograms of logical material amounts.

Five, the band middle layer of the present invention's design and the extruding of the wearing layer extruding pin of one of tool and mould, this extruding pin is by with 3Cr2W8V and 4Cr5MoVlSi and high Cr, Mo, a kind of in Mn steel alloy and this class material after surfaces nitrided processing is base material, the titanium nitride middle layer that high nitrogen is arranged outside base material, titanium nitride coating outside the middle layer is formed. and the nitrogen content of the titanium nitride in middle layer is in the 95-115at% scope, its thickness is the 0.1-1 micron, the composition of outermost titanium nitride is near stoichiometry. after the extruding pin cleans through general chemical physics earlier, place depositing device, be evacuated down to about 1 * 10 earlier ^-2Pa,

Being heated to outgases in the 350-590 ℃ of temperature range to reach carries out surface activation process under argon gas atmosphere, under the high pressure of 500-1500 volt scope, bombard workpiece surface through Ionized argon gas, after about 10-20 minute base material covered to enter and give deposition procedures, promptly obtain the middle layer in the workpiece surface deposition. when giving deposition, remove high pressure earlier, and workpiece applied negative bias Ub, the gas total pressure is 0.1-1.6Pa, the ratio of the partial pressure of reactant gases (nitrogen) and working gas (argon gas) is the partial pressure that the partial pressure of 1-7. reactant gases is higher than working gas all the time, nitrogen content in the titanium nitride that generates is higher than stoichiometric quantity, thereby, nitrogen wherein increases combining between middle layer and the workpiece so that infiltrating the workpiece base material gradually in subsequent handling. gas total pressure when giving deposition, partial pressure is strong, base material temperature and negative bias are seen Fig. 1 to the influence of base material and middle layer bonding force, 2,3,4. when depositing, the gas total pressure is 0.07-1.2Pa, the partial pressure 0.03-0.6Pa of working gas argon, the partial pressure of reactant gases nitrogen remains on 0.03-0.6Pa, promptly finish through 20-50 minute deposition approximately. be cooled to after covering below 250 ℃ and can come out of the stove. processing parameter is seen Fig. 5 to the influence of coating microhardness during deposition, 6,7,8, Fig. 9 is seen in the influence of friction durability, 10,11, do not see Figure 13 12. there is the wear curve of the sample of the sample of the 3Cr2W8V of top coat and two kinds of die steel of 4Cr5MoVlSi and band coating of the present invention. coating structure is FCC-TiN(δ).

Measured the various normal temperature mechanical properties (tensile strength sigma b. unit elongation δ, reduction of area) of coating sample and contrasted with other samples, it the results are shown in Figure the 14-16. high-temperature mechanical property and sees that Figure 17-19. result shows that the TiN coating does not influence the tensile strength of mould steel, unit elongation and relative reduction in area, though also do not change the high-temperature mechanical behavior of base material. and improving surface hardness, nitriding treatment significantly reduces mechanical property.

Totally 90 extruding pins with the not coating of same size of make four batches extruding of present embodiment pins contrasts use and show in aluminum pipe production, coating extruding pin is significantly improved aluminum pipe inwall quality, and the scratch scrap rate drops to 2.45%. by 6.39% ten kinds of alloys statistics of 163 batches of three kinds of specifications tubing integrated yield be the results are shown in Table 5.

The extruding pin matrix metal aluminium of producing proof band TiN coating is far fewer than coating pin not, so can significantly reduce high temperature sand pin, the number of times that is coated with lubricant and degree before the extruding, thereby enhance productivity and improve working conditions. calculate with annual 800 tons of aluminum pipe finished products, need to drop into nearly 1476 tons of metal aluminium ingots by former yield rate calculating, and after using band TiN coating extruding pin, can under the condition that does not increase material, water power, consumption, manpower, equipment attrition and communications and transportation, increase

About 84.7 tons of product tubing. in other words to finish 800 tons of tubing, use coating extruding pin only need drop into 1334.5 tons of aluminium ingots, save metal more than 141 tons.

Six, identical with embodiment five, tool and mould also is made up of base material, middle layer and coating, difference is that base material is the W48Cr4V rapid steel. and the depositing operation of middle layer and coating is identical with example five. and the gained tool and mould is particularly suitable for extruding plastic tubing. and the wear resistance of tool and mould, base material and coating's adhesion satisfy the requirement of plastics extrusion molding fully, and coating is incrust.

Seven, the composition and the coating process of extruding pin are identical with example five, difference is to also have the back deposition procedures after deposition procedures. when carrying out the back deposition procedures, the dividing potential drop of reactant gases nitrogen is adjusted to 0.05-0.5Pa, got final product through 2.5 minutes the top layer that surface tinted is more beautiful, hardness is higher, its microhardness can reach more than the 35GPa.

Eight. the composition and the coating process of extruding pin are identical with example five, difference is that the extruding pin is installed on the device shown in Figure 20, makes the extruding pin can translation in giving operations such as deposition, deposition and the planet rotation. the unevenness of the extruding wire surface coat-thickness of making is less than ± 4%.

The processing parameter that gives deposition and deposition procedures is: 160 volts of negative biass, 450 ℃ of base material temperatures, give sedimentary gas total pressure 0.3Pa, the strong 0.18Pa of nitrogen partial pressure, the strong 0.12Pa of partial pressure of ar gas, sedimentation velocity per second 15 dusts, gave deposition 5 minutes. the gas total pressure 0.6Pa during deposition, the strong 0.3Pa of nitrogen partial pressure, the strong 0.3Pa of partial pressure of ar gas, sedimentation velocity per second 50 dusts, deposit 20 minutes. measuring its microhardness of coating is 30GPa, bonding force Lc50N. does not find disbonding through 1000 extruded aluminum tubes, the not sticking aluminium knurl in surface.

Nine. the extruding tool and mould of the present invention's design is prod cast, various cores etc. and its composition is identical with example five with technology. and positive effect is arranged in the use equally, and coating is not peeled off, not sticking aluminium.

Claims (6)

1, a kind of hot extrusion tool and mould of being made up of base material, wear-resistant coating in the middle layer on the base material, on the middle layer is characterized in that:

What [1] said base material was various hot extrusion tool and moulds with in steel, the rapid steel is a kind of;

[2] said middle layer is that nitrogen content is higher than stoichiometric high nitrogen titanium nitride layer, and its thickness is the 0-1 micron,

[3] said coating is that composition is near stoichiometric titanium nitride layer.

2, a kind of by the manufacture method of the said hot extrusion of claim 1 with tool and mould, said manufacture method comprises substrate surface treatment, deposition procedures, substrate surface treatment comprises that the chemical physics on surface is cleaned, the degassing and ion bombardment surface activation process under vacuum, said surface deposition operation adopts physical vaporous deposition, it is characterized in that:

The processing condition of said deposition procedures are: base material temperature Ts350-590 ℃, negative bias Ub0-240 volt, at gas total pressure 0.07-1.2Pa, the partial pressure 0.03-0.6Pa of working gas argon, under the condition of the partial pressure 0.03-0.6Pa of reactant gases nitrogen, molten metal titanium tetrachloride vapor and nitrogen reaction generate titanium nitride coating, sedimentation velocity per second 5-80 dust in the substrate surface deposition.

3, by the manufacture method of the said hot extrusion of claim 2 with tool and mould, it is characterized in that giving the processing back on the surface also has the surface to give deposition procedures, the processing condition that deposition procedures is given on said surface are: base material temperature Ts350-590 ℃, negative bias Ub0-240 volt, at gas total pressure 0.1-1.6Pa, the partial pressure 0.04-0.8Pa of working gas argon, the partial pressure 0.04-1.0Pa of reactant gases nitrogen, the partial pressure of reactant gases nitrogen is under the condition of 1-7 with the ratio β of the partial pressure of working gas argon, the steam of molten metal titanium and nitrogen are reflected at the titanium nitride inter coat that the substrate surface deposition generates high nitrogen-containing, sedimentation velocity per second 5-80 dust.

4, according to the manufacture method of the said extruding of claim 3 with tool and mould, when it is characterized in that giving deposition procedures and deposition procedures on the surface activation process of carrying out said base material, surface, translation done by base material and planet rotates.

5,, it is characterized in that covering operation in addition after the said surface activation process operation and after the deposition procedures according to the manufacture method of the said extruding of claim 4 with tool and mould.

6, according to the manufacture method of the said extruding of claim 5 with tool and mould, it is characterized in that after said deposition procedures, also having the back deposition procedures, its mode of deposition is 0.1-0.8Pa for the gas total pressure, the partial pressure of working gas argon is 0.05-0.4Pa, the partial pressure 0.05-0.5Pa. of reactant gases nitrogen

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