CN104862652A - Method for manufacturing TiAlSiN super-hard gradient coating - Google Patents
Method for manufacturing TiAlSiN super-hard gradient coating Download PDFInfo
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- CN104862652A CN104862652A CN201510237876.2A CN201510237876A CN104862652A CN 104862652 A CN104862652 A CN 104862652A CN 201510237876 A CN201510237876 A CN 201510237876A CN 104862652 A CN104862652 A CN 104862652A
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Abstract
The invention provides a method for manufacturing a TiAlSiN super-hard gradient coating. The method includes the steps that abrasive blasting and cleaning are carried out on the surface of a workpiece; the step of plating the TiAlSiN super-hard gradient coating on the workpiece through a cathode ion plating process includes the first stage of manufacturing a Ti prime coating, the second stage of manufacturing a TiN gradient coating, the third stage of manufacturing a TiAl gradient coating, the fourth stage of manufacturing a TiAlN gradient coating, the fifth stage of manufacturing a SiN gradient coating and the sixth stage of manufacturing a TiSi gradient coating; finally, the surfaces of the coatings are polished. The elasticity modulus of the TiAlSiN gradient coating manufactured through the method can reach 340 GPa, high-temperature-resistant oxidation temperature can reach 1200 DEG C, high-speed cutting of quenched steel and other workpieces with the hardness over HRC60 can be achieved, and the service life of a cutter is greatly prolonged.
Description
Technical field
The invention belongs to materialogy field, relate to a kind of process for modifying surface of metal-cutting machine tool, specifically a kind of preparation method with the superhard gradient cladding of superhard, high temperature resistant, oxidation resistant TiAlSiN.
Background technology
Physical vapor deposition (Physical Vapor Deposition, PVD) be that one adopts physical method under vacuum, gaseous atom, molecule or partial ionization is become to become ion solid or fluent material surface vaporization, and by low-pressure gas (or plasma body) process, there is in matrix surface deposition the technology of certain specific function film, specifically comprise vacuum evaporation, sputtering plating and ion plating.Cathode ion plating has evaporation and sputters the advantage of plating, and is therefore applied to the coating preparation of high rigidity more and more widely.Traditional binary coating, ternary coating are as CrN, TiC, (Ti, Al) N, TiCN etc. also have very large help to the raising of cutter life, but along with the further raising of processing request, new coating material and preparation technology be corresponding birth also, as compound coatings such as TiSiCN, TiSiCoN, TiAlSiCN.
TiAlSiN coating is compared TiAlN coating, and adding of Si element makes it have higher hardness, wear resistance and high-temperature stability.Si element add the effect with crystal grain thinning, because of Si be insoluble to TiAlN crystalline substance bag, amorphous Si
3n
4be positioned at the grain boundaries of TiAlN phase mutually, suppress the growth of crystal grain, improve hardness, the wear resistance of coating, form Si
3n
4the composite structure of mutually coated TiAlN.TiAlSiN coating is described as the superhard coating of a new generation, and by changing preparation technology, optimized coatings parameter, the TiAlSiN coating that the content processability of change Si element and other elements is more excellent is the focus that current educational circles is studied.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides the preparation method of the superhard gradient cladding of a kind of TiAlSiN, the preparation method of the described superhard gradient cladding of this TiAlSiN solves metal working tool of the prior art due to hardness, poor high temperature stability and cause cutting-tool's used life not reach the technical problem of requirement.
The preparation method of the superhard gradient cladding of a kind of TiAlSiN of the present invention, comprises the following steps:
1) one is carried out the step of sandblasting to workpiece surface, is put in by workpiece in sand-blast device, and opening device carries out sandblasting to workpiece surface, removes the oxide skin on surface, dirt, erosion and impurity thereof;
2) step of cleaning workpiece, carries out the cleaning of workpiece surface by the alcohol that first utilizes through sandblasting, and recycling ultrasonic wave is cleaned workpiece surface, is finally processed workpiece surface by plasma process again;
3) step adopting cathode ion depositing process workpiece to be coated with to the superhard gradient cladding of TiAlSiN, wherein, vacuum chamber temperature controls between 400-500 DEG C, maintenance vacuum tightness is 0.005-0.06mbar, nitrogen flow is 150-220sccm, by six stages, the superhard gradient cladding of TiAlSiN is coated with to workpiece, first stage is that Ti prepares prime coat layer, argon gas (Ar) is passed in vacuum furnace chamber, Ar flow is 180-230sccm, Ti target is energized deposit, electrical current is 120-150A, bias voltage is 400-500V, vacuum tightness is 0.008mbar, depositing time is 30s-120s, subordinate phase is preparation TiN gradient cladding, stops passing into Ar, opens N
2flow valve passes into N in vacuum furnace chamber
2, N
2flow is 150-200sccm, and makes Ti target continue to keep the switch-on regime in the first stage, and electrical current is 120-150A, and bias voltage is 100-130V, and vacuum tightness is 0.007mbar, and depositing time is 6-8min, obtains the TiN coating that Ti content increases progressively, phase III is preparation TiAl gradient cladding, stops passing into N in vacuum furnace chamber
2in furnace chamber, pass into Ar simultaneously, Ar flow is 180-230sccm, make AlTi target and the energising of Ti target, AlTi target electrical current is 120-160A, Ti target electrical current is 120-150A, bias voltage is 100-120V, vacuum tightness is 0.01-0.02mbar, and depositing time is 20-30min, obtains the gradient cladding containing Al, fourth stage is preparation TiAlN gradient cladding, stops passing into Ar in vacuum furnace chamber, continues to pass into N in furnace chamber
2, N
2flow is 180-200sccm, continues to make AlTi target and Ti target be in switch-on regime, and AlTi target electrical current is 150-180A, Ti target electrical current is 120-150A, and bias voltage is 40-60V, and vacuum tightness is 0.01-0.02mbar, depositing time is 1.5h, obtains the TiAlN coating that Al content increases progressively, five-stage is preparation TiAlSiN gradient cladding, and the power-off of Ti target, continues to pass into N in furnace chamber
2, N
2flow is 180-250sccm, and continues to make AlTi target be in switch-on regime, and electrical current is 150-180A, makes SiTi target be energized simultaneously, and electrical current is 120-160A, and bias voltage is 60-80V, and vacuum tightness is 0.04-0.06mbar, and depositing time is 42min, 6th stage was that TiSiN prepares gradient cladding, and SiTi target continues to keep switch-on regime, and Ti target and the power-off of AlTi target, electrical current is 140-160A, continues to pass into N in furnace chamber
2, N
2flow is 180-200sccm, and bias voltage is 60-80V, and vacuum tightness is 0.04-0.05mbar, and depositing time is 20min,
4) one is carried out the step of polished finish to TiAlSiN gradient cladding, by prepare have TiAlSiN gradient cladding clamping workpiece and polishing machine on, start polishing machine, and set polishing time and polishing velocity, start polishing program and carry out polishing.
Further, be 20:80 for the mass ratio that the purity of Ti target in depositing Ti AlSiN gradient cladding target used is 99.999%, the mass ratio of Al and Ti is Si and Ti in 70:30, SiTi target in AlTi target.
Further, arranging polishing time is 10 ~ 20min, and polishing velocity is for being 8 ~ 15m/s.
Further, the thickness of described TiAlSiN gradient cladding is one side 2.5-3.5 μm.
Further, in step workpiece surface processed by plasma process, clamping workpiece is sent into the coating furnace chamber of preheating, start-up routine, after furnace chamber vacuumizes and workpiece temperature reaches 400-500 DEG C time, pass into argon gas (Ar), flow is 180-230sccm, and arranging bias voltage is 700-950V, and vacuum tightness is 0.005-0.008mbar, carry out plasma cleaning to workpiece, scavenging period is 10 ~ 30min.
The present invention adopts gradient cladding technology, effectively can alleviate the larger unrelieved stress caused because material character is different between coated material from matrix, makes to have good bonding force between coating and matrix and gradient cladding.Carry out polished finish to the matrix after coating, arranging polishing time is 10 ~ 20min, and polishing velocity, not only can the drop of matrix surface after decoating for being 8 ~ 15m/s, can also play the effect of strengthening by effects on surface.The thickness of TiAlSiN gradient cladding prepared by the present invention is one side 2.5-3.5 μm, Young's modulus can reach 340GPa, high temperature oxidation resisting temperature can reach more than 1200 DEG C, can realize being that the workpiece such as hardened steel of more than HRC60 carries out High Speed Machining to hardness, increase substantially cutting-tool's used life.
The present invention, compared with existing Technology, has the following advantages:
(1) the TiAlSiN gradient cladding that prepared by the present invention has excellent high temperature oxidation resistance, finds its high-temperature stable Ding Keda more than 1200 DEG C through high temperature resistant test.
(2) the TiAlSiN gradient cladding prepared of the present invention due to Al element under the high temperature conditions can with O
2reaction generates fine and close oxide film, effectively can alleviate the erosion of material inside oxidized and external reaction element further; In coating Si and Al element for surface oxidized and formed TiO
2there is restraining effect from Anatase to the transformation of rutile, hinder the carrying out of oxidation.
(3) the TiAlSiN gradient cladding that prepared by the present invention has excellent mechanical property, can realize carrying out High Speed Machining to workpiece such as the hardened steel to hardness being more than HRC60; The interpolation of Si element, has the effect of crystal grain thinning, and coating hardness is increased, and wear resistance is corresponding improve also.
(4) the TiAlSiN gradient cladding prepared of the present invention is because adopting gradient cladding form, contributes to alleviating the mechanical stress and thermal stresses that are coated with interlayer, makes coating have good toughness and heat resistanceheat resistant vibrations performance, have good bonding force simultaneously between coating and matrix.
(5) the TiAlSiN gradient cladding of the present invention to preparation carries out polished finish, can remove the drop on surface, can also play the effect of coatingsurface strengthening.
(6) adopt cathode ion coating technology to prepare TiAlSiN gradient cladding under lower depositing temperature, can not damage coated matrix; The accurate control to coated component can be realized by control target current, bias voltage and nitrogen flow.
(7) the TiAlSiN gradient cladding of the present invention to preparation proves through cutting test, can increase substantially the work-ing life of cutting tool, save production cost, increase economic efficiency.
The present invention compares with prior art, and its technical progress is significant.The present invention adopts cathode ion coating technology to deposit, and cathode ion plating combines the advantage of vacuum evaporation and sputtering plating, and particle is good around plating property, and energy is high, and rate of ionization is high, and make the coating dense uniform prepared, hardness is high.This gradient cladding can increase substantially the surface hardness of cutter, high temperature oxidation resistance and work-ing life, has better toughness, abrasion resistance and high-temperature oxidation, improve production efficiency than non-coated tool.
Accompanying drawing explanation
Fig. 1 compares in two kinds of coatings cutting high hard material life-spans.
Embodiment
Embodiment 1
The preparation method of the superhard gradient cladding of a kind of TiAlSiN of the present invention, comprises the following steps:
(1) workpiece surface sandblasting and cleaning
Be put in by matrix in sand-blast device, opening device carries out sandblasting to workpiece surface, removes the oxide skin on surface, dirt, erosion and impurity thereof.After sandblasting terminates, take out workpiece, recycling alcohol manually carries out workpiece surface cleaning, removes the residuals such as the greasy dirt on surface.After treating manual cleaning, workpiece is carried out clamping and sends in Ultrasonic Cleaners utilize ultrasonic wave automatically to clean.Ultrasonic cleaning completes and after drying workpiece, clamping workpiece is sent into the coating furnace chamber of preheating, start-up routine, after furnace chamber vacuumizes and substrate temperature reaches 400-500 DEG C, pass into argon gas (Ar), flow is 180-230sccm, arranging bias voltage is 700-950V, vacuum tightness is 0.005-0.008mbar, carries out plasma cleaning to workpiece, and scavenging period is 15min.
(2) preparation of the superhard gradient cladding of TiAlSiN
Adopt cathode ion coating technology to be coated with the superhard gradient cladding of TiAlSiN to matrix under UHV condition, vacuum chamber temperature controls at 400-500 DEG C, and maintenance vacuum tightness is 0.005-0.06mbar, nitrogen (N
2) flow is 150-220sccm, the target that different coating phase is corresponding, bias voltage, target current are different.
A. the preparation of first stage Ti prime coat layer.Continue to pass into argon gas (Ar) in vacuum furnace chamber, Ar flow is 180-230sccm, and Ti target is energized and deposits, electrical current is 120-150A, and bias voltage is 400-500V, and vacuum tightness is 0.008mbar, and depositing time is 30s-120s.
B. the preparation of subordinate phase TiN gradient cladding.Stop passing into Ar, open N
2flow valve passes into N in vacuum furnace chamber
2, N
2flow is 150-200sccm, and makes Ti target continue to keep the switch-on regime in a, and electrical current is 120-150A, and bias voltage is 100-130V, and vacuum tightness is 0.007mbar, and depositing time is 6-8min, obtains the TiN coating that Ti content increases progressively.
C. the preparation of phase III TiAl gradient cladding.Stop passing into N in vacuum furnace chamber
2in furnace chamber, pass into Ar simultaneously, Ar flow is 180-230sccm, make AlTi target and the energising of Ti target, AlTi target electrical current is 120-160A, Ti target electrical current is 120-150A, bias voltage is 100-120V, vacuum tightness is 0.01-0.02mbar, and depositing time is 20-30min, obtains the gradient cladding containing Al.
D. the preparation of fourth stage TiAlN gradient cladding.Contrary with step c, now stop passing into Ar in vacuum furnace chamber, continue to pass into N in furnace chamber
2, N
2flow is 180-200sccm, continues to make AlTi target and Ti target be in switch-on regime, and AlTi target electrical current is 150-180A, Ti target electrical current is 120-150A, and bias voltage is 40-60V, and vacuum tightness is 0.01-0.02mbar, depositing time is 1.5h, obtains the TiAlN coating that Al content increases progressively.
E. the preparation of five-stage TiAlSiN gradient cladding.The power-off of Ti target, continues to pass into N in furnace chamber
2, N
2flow is 180-250sccm, and continues to make AlTi target be in switch-on regime, and electrical current is 150-180A, makes SiTi target be energized simultaneously, and electrical current is 120-160A, and bias voltage is 60-80V, and vacuum tightness is 0.04-0.06mbar, and depositing time is 42min.
F. the preparation of the 6th stage TiSiN gradient cladding.SiTi target continues to keep switch-on regime, and all the other target power-off, electrical current is 140-160A, continues to pass into N in furnace chamber
2, N
2flow is 180-200sccm, and bias voltage is 60-80V, and vacuum tightness is 0.04-0.05mbar, and depositing time is 20min.
(3) polished finish is carried out to TiAlSiN gradient cladding
By prepare have TiAlSiN gradient cladding matrix clamping and polishing machine on, start polishing machine, and set polishing time and polishing velocity, start polishing program and carry out polishing.
In technique scheme, be Ti target (purity is 99.999%), AlTi target (W for the target that depositing Ti AlSiN gradient cladding is used
al: W
ti=70:30) and SiTi target (W
si: W
ti=20:80).
In technique scheme, carry out polished finish to the matrix after coating, arranging polishing time is 15min, and polishing velocity is 10m/s, not only can the drop of matrix surface after decoating, can also play the effect of strengthening by effects on surface.
In technique scheme, the thickness of the TiAlSiN gradient cladding of preparation is one side 2.5-3.5 μm, and Young's modulus can reach 340GPa, and high temperature oxidation resisting temperature can reach more than 1200 DEG C.In technique scheme, the thickness of the TiAlSiN gradient cladding of preparation is one side 2.5-3.5 μm, and Young's modulus can reach 340GPa, and high temperature oxidation resisting temperature can reach more than 1200 DEG C.
The high temperature resistant experiment of embodiment 2 TiAlSiN
Select 5 groups, rapid steel (trade mark M2) sample, often organize 5 (every sheet specification Φ 20 × 5), by a mirror polish of sample, carry out TiAlSiN coating according to above technique after whole sample cleaning, the one side thickness of coating is all 3 microns.The coating sample prepared is put into process furnace respectively by group, the temperature of setting process furnace is 600 DEG C, 800 DEG C, 1000 DEG C, 1200 DEG C and 1400 DEG C respectively, then cut by sample with slow wire feeding, under scanning electron microscope, observe cross section, coating position situation, result is as shown in table 1.
table 1 high temperature experiment scanning electron microscopic observation result
The high rigidity cutting experiment of embodiment 3 TiAlSiN coating
Cutter: Wimet bulb milling cutter, Φ 10mm;
Machined material: Japanese Datong District die steel DC53, hardness HRC60;
Cutting parameter: v=320m/min;
f=0.2mm/r；
a
p=0.3mm；
VB=0.12mm；
The type of cooling: DRY CUTTING;
With reference to coating: Switzerland's commodity coating;
Select Wimet bulb milling cutter in the present embodiment, carry out high rigidity milling test by TiAlSiN coating.Have Switzerland Co., Ltd's specialty to prepare milling cutter high rigidity in the market and cut coating, in order to compare, the special coating of this Switzerland Co., Ltd of family production and the TiAlSiN coating selected compares.By the coating called after " Switzerland's commodity coating " that Switzerland Co., Ltd produces.Experimental result as shown in Figure 1.Result can be found out by experiment, TiAlSiN coating is under identical experiment condition, and milling matrix hardness is the material of HRC60, and milling length reaches 880 meters, and a current commercial Switzerland commodity coating milling 430 meters.Experimental result shows, the life-span of TiAlSiN coating in hard machining is far away higher than commercial hard machining coating on the market.
Claims (5)
1. a preparation method for the superhard gradient cladding of TiAlSiN, is characterized in that comprising the following steps:
One is carried out the step of sandblasting to workpiece surface, is put in by workpiece in sand-blast device, and opening device carries out sandblasting to workpiece surface, removes the oxide skin on surface, dirt, erosion and impurity thereof;
A step of cleaning workpiece, carries out the cleaning of workpiece surface by the alcohol that first utilizes through sandblasting, and recycling ultrasonic wave is cleaned workpiece surface, is finally processed workpiece surface by plasma process again;
A step adopting cathode ion depositing process workpiece to be coated with to the superhard gradient cladding of TiAlSiN, wherein, vacuum chamber temperature controls between 400-500 DEG C, maintenance vacuum tightness is 0.005-0.06mbar, nitrogen flow is 150-220sccm, by six stages, the superhard gradient cladding of TiAlSiN is coated with to workpiece, first stage is that Ti prepares prime coat layer, argon gas is passed in vacuum furnace chamber, Ar flow is 180-230sccm, Ti target is energized deposit, electrical current is 120-150A, bias voltage is 400-500V, vacuum tightness is 0.008mbar, depositing time is 30s-120s, subordinate phase is preparation TiN gradient cladding, stops passing into Ar, opens N
2flow valve passes into N in vacuum furnace chamber
2, N
2flow is 150-200sccm, and makes Ti target continue to keep the switch-on regime in the first stage, and electrical current is 120-150A, and bias voltage is 100-130V, and vacuum tightness is 0.007mbar, and depositing time is 6-8min, obtains the TiN coating that Ti content increases progressively, phase III is preparation TiAl gradient cladding, stops passing into N in vacuum furnace chamber
2in furnace chamber, pass into Ar simultaneously, Ar flow is 180-230sccm, make AlTi target and the energising of Ti target, AlTi target electrical current is 120-160A, Ti target electrical current is 120-150A, bias voltage is 100-120V, vacuum tightness is 0.01-0.02mbar, and depositing time is 20-30min, obtains the gradient cladding containing Al, fourth stage is preparation TiAlN gradient cladding, stops passing into Ar in vacuum furnace chamber, continues to pass into N in furnace chamber
2, N
2flow is 180-200sccm, continues to make AlTi target and Ti target be in switch-on regime, and AlTi target electrical current is 150-180A, Ti target electrical current is 120-150A, and bias voltage is 40-60V, and vacuum tightness is 0.01-0.02mbar, depositing time is 1.5h, obtains the TiAlN coating that Al content increases progressively, five-stage is preparation TiAlSiN gradient cladding, and the power-off of Ti target, continues to pass into N in furnace chamber
2, N
2flow is 180-250sccm, and continues to make AlTi target be in switch-on regime, and electrical current is 150-180A, makes SiTi target be energized simultaneously, and electrical current is 120-160A, and bias voltage is 60-80V, and vacuum tightness is 0.04-0.06mbar, and depositing time is 42min, 6th stage was that TiSiN prepares gradient cladding, and SiTi target continues to keep switch-on regime, and Ti target and the power-off of AlTi target, electrical current is 140-160A, continues to pass into N in furnace chamber
2, N
2flow is 180-200sccm, and bias voltage is 60-80V, and vacuum tightness is 0.04-0.05mbar, and depositing time is 20min,
One is carried out the step of polished finish to TiAlSiN gradient cladding, by prepare have TiAlSiN gradient cladding clamping workpiece and polishing machine on, start polishing machine, and set polishing time and polishing velocity, start polishing program and carry out polishing.
2. as claimed in claim 1, the preparation method of the superhard gradient cladding of a kind of TiAlSiN, it is characterized in that: be 20:80 for the mass ratio that the purity of Ti target in the target that depositing Ti AlSiN gradient cladding is used is 99.999%, the mass ratio of Al and Ti is Si and Ti in 70:30, SiTi target in AlTi target.
3. as claimed in claim 1, the preparation method of the superhard gradient cladding of a kind of TiAlSiN, is characterized in that: arranging polishing time is 10 ~ 20min, and polishing velocity is for being 8 ~ 15m/s.
4. as claimed in claim 1, the preparation method of the superhard gradient cladding of a kind of TiAlSiN, is characterized in that: the thickness of described TiAlSiN gradient cladding is one side 2.5-3.5 μm.
5. as claimed in claim 1, the preparation method of the superhard gradient cladding of a kind of TiAlSiN, it is characterized in that: in step workpiece surface processed by plasma process, clamping workpiece is sent into the coating furnace chamber of preheating, start-up routine, after furnace chamber vacuumizes and workpiece temperature reaches 400-500 DEG C time, pass into argon gas, flow is 180-230sccm, arranging bias voltage is 700-950V, vacuum tightness is 0.005-0.008mbar, carries out plasma cleaning to workpiece, and scavenging period is 10 ~ 30min.
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