CN104862652B - Method for manufacturing TiAlSiN super-hard gradient coating - Google Patents
Method for manufacturing TiAlSiN super-hard gradient coating Download PDFInfo
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- CN104862652B CN104862652B CN201510237876.2A CN201510237876A CN104862652B CN 104862652 B CN104862652 B CN 104862652B CN 201510237876 A CN201510237876 A CN 201510237876A CN 104862652 B CN104862652 B CN 104862652B
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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, it is related to a kind of process for modifying surface of metal-cutting machine tool, specifically one
Kind there is superhard, high temperature resistant, the superhard gradient coating of oxidation resistant tialsin preparation method.
Background technology
Physical vapour deposition (PVD) (physical vapor deposition, pvd) is that one kind adopts thing under vacuum
Reason method, solid or fluent material surface vaporization are become gaseous atom, molecule or partial ionization to become ion, and pass through low-pressure gas
(or plasma) process, has the technology of certain specific function film, specifically includes vacuum evaporation, splashes in matrix surface deposition
Penetrate plating and ion plating.Cathode ion plating has the advantages that evaporation and sputtering plating, is therefore more and more widely applied to high rigidity
Coating preparation.Traditional binary coating, ternary coating such as crn, tic, the raising to cutter life for (ti, al) n, the ticn etc.
There is very big help, but the raising further with processing request, new coating material and preparation technology also corresponding birth
Raw, the such as composite coating such as tisicn, tisicon, tialsicn.
Tialsin coating compares for tialn coating, and the addition of si element makes it have higher hardness, wearability
And high-temperature stability.The addition of si element has the effect of crystal grain thinning, because si does not dissolve in the brilliant bag of tialn, amorphous si3n4Phase place
In the grain boundaries of tialn phase, suppress the growth of crystal grain, improve hardness, the wearability of coating, form si3n4Mutually coat tialn's
Composite construction.Tialsin coating is described as the superhard coating of a new generation, by changing preparation technology, optimizes coating parameter, changes
The tialsin coating that the content processability of si element and other elements is more excellent is the focus that current educational circles is studied.
Content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of system of the superhard gradient coating of tialsin
Preparation Method, the preparation method of the described superhard gradient coating 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.
A kind of preparation method of the superhard gradient coating of tialsin of the present invention, comprises the following steps:
1) step carrying out sandblasting to surface of the work, workpiece is put in abrasive blast equipment, and equipment of opening is to workpiece table
Face carries out blasting treatment, removes oxide skin, dirt, erosion and its impurity on surface；
2) step that workpiece is carried out, will carry out the clear of surface of the work through blasting treatment first with alcohol
Wash, recycle ultrasonic wave that surface of the work is carried out, finally by plasma process, surface of the work is processed again；
3) step that using cathode ion depositing process, workpiece is coated with the superhard gradient coating of tialsin, wherein, vacuum
Room temperature controls between 400-500 DEG C, and holding vacuum is 0.005-0.06mbar, and nitrogen flow is 150-220sccm,
By six stages, workpiece is coated with the superhard gradient coating of tialsin, the first stage prepares prime coat layer for ti, to vacuum furnace chamber
In be passed through argon gas (ar), ar flow be 180-230sccm, make ti target be energized deposited, electrical current be 120-150a, bias
Voltage is 400-500v, and vacuum is 0.008mbar, and sedimentation time is 30s-120s；Second stage is that preparation tin gradient applies
Layer, stops being passed through ar, opens n2Flow valve is passed through n into vacuum furnace chamber2, n2Flow is 150-200sccm, and so that ti target is continued
Keep the "on" position in the first stage, electrical current is 120-150a, bias voltage is 100-130v, vacuum is
0.007mbar, sedimentation time is 6-8min, obtains the tin coating that ti content is incremented by；Phase III is that preparation tial gradient applies
Layer, stops being passed through n in vacuum furnace chamber2, it is passed through ar in furnace chamber, ar flow is 180-230sccm, makes alti target and ti simultaneously
Target is energized, and alti target electrical current is 120-160a, and ti target electrical current is 120-150a, and bias voltage is 100-120v, very
Reciprocal of duty cycle is 0.01-0.02mbar, and sedimentation time is 20-30min, obtains the gradient coating containing al；Fourth stage is preparation tialn
Gradient coating, stops being passed through ar in vacuum furnace chamber, continues to be passed through n in furnace chamber2, n2Flow is 180-200sccm, continues to make
Alti target and ti target are in "on" position, and alti target electrical current is 150-180a, and ti target electrical current is 120-150a, biasing
Voltage is 40-60v, and vacuum is 0.01-0.02mbar, and sedimentation time is 1.5h, obtains the tialn coating that al content is incremented by；
5th stage was preparation tialsin gradient coating, and ti target power-off continues to be passed through n in furnace chamber2, n2Flow is 180-250sccm,
And continue to make alti target be in "on" position, electrical current is 150-180a, so that siti target is energized simultaneously, and electrical current is 120-
160a, bias voltage is 60-80v, and vacuum is 0.04-0.06mbar, and sedimentation time is 42min；6th stage was tisin system
Standby gradient coating, siti target continues to remain powered on state, ti target and alti target power-off, and electrical current is 140-160a, continue to
It is passed through n in furnace chamber2, n2Flow is 180-200sccm, and bias voltage is 60-80v, and vacuum is 0.04-0.05mbar, during deposition
Between be 20min；
4) step that tialsin gradient coating is processed by shot blasting, has been prepared and has been had tialsin gradient coating
On clamping workpiece and polishing machine, start polishing machine, and set polishing time and polishing velocity, start polishing program and thrown
Light.
Further, the purity for depositing ti target in the target used by tialsin gradient coating is 99.999%, alti
In target, the mass ratio of al and ti is 70:30, and in siti target, the mass ratio of si and ti is 20:80.
Further, setting polishing time is 10 ~ 20min, and polishing velocity is 8 ~ 15m/s.
Further, the thickness of described tialsin gradient coating is 2.5-3.5 μm of one side.
Further, in step surface of the work being processed by plasma process, by clamping workpiece simultaneously
Send into warmed-up coating furnace chamber, startup program, after furnace chamber vacuumizes and when workpiece temperature reaches 400-500 DEG C, be passed through argon
Gas (ar), flow is 180-230sccm, and setting bias is 700-950v, and vacuum is 0.005-0.008mbar, and workpiece is entered
Row plasma cleaning, scavenging period is 10 ~ 30min.
The present invention adopts gradient coating technology, can effectively alleviate between coating material and matrix because material character is different
The larger residual stress causing is well bonded so that having between coating and matrix and gradient coating.To the base after coating
Body is processed by shot blasting, setting polishing time is 10 ~ 20min, and polishing velocity is 8 ~ 15m/s, not only can remove removing coating
The drop of matrix surface afterwards, can also play the effect of strengthening to surface.The thickness of the tialsin gradient coating of present invention preparation
For 2.5-3.5 μm of one side, up to 340gpa, high temperature oxidation resisting temperature, up to more than 1200 DEG C, can achieve to hardness elastic modelling quantity
The workpiece such as the hardened steel for more than hrc60 carry out high-speed cutting processing, and cutting-tool's used life is greatly improved.
The present invention, compared with existing process technology, has the advantage that
(1) the tialsin gradient coating of present invention preparation has excellent high temperature oxidation resistance, finds through high temperature resistant test
Its high-temperature stable is determined up to more than 1200 DEG C.
(2) present invention preparation tialsin gradient coating due to al element under the high temperature conditions can be with o2Reaction generates
Fine and close oxide-film, can effectively alleviate that internal material is oxidized further and the erosion of external reaction element；In coating
The tio that si and al element is oxidized for surface and is formed2There is inhibitory action from Anatase to the transformation of rutile, hinder oxygen
The carrying out changing.
(3) present invention preparation tialsin gradient coating there is excellent mechanical property, can achieve to hardness be
The workpiece such as the hardened steel of more than hrc60 carry out high-speed cutting processing；The interpolation of si element, has the effect of crystal grain thinning, makes painting
Layer hardness increases, and wearability also accordingly improves.
(4) the tialsin gradient coating of present invention preparation is because using gradient coating form, contributing to alleviating the machine applying interlayer
Tool stress and thermal stress, so that coating has good toughness and heat resistanceheat resistant vibrations performance, have good simultaneously between coating and matrix
Good adhesion.
(5) present invention is processed by shot blasting to the tialsin gradient coating of preparation, can remove the drop on surface, also may be used
To play the effect of coating surface strengthening.
(6) tialsin gradient coating is prepared under relatively low depositing temperature using cathode ion coating technology, will not be to being applied
Layer matrix damages；The accurate control to coating composition can be realized by controlling target current, bias voltage and nitrogen flow
System.
(7) present invention proves to the resected test of tialsin gradient coating of preparation, can increase substantially cutting tool
Service life, save production cost, increase economic efficiency.
The present invention compares with prior art, and its technological progress is significant.The present invention is carried out using cathode ion coating technology
Deposition, cathode ion plating combines vacuum evaporation and the advantage of sputtering plating, and particle is good around plating property, and energy is high, and rate of ionization is high, makes
The coating dense uniform that must prepare, hardness is high.This gradient coating can increase substantially the case hardness of cutter, high temperature oxidation resistance
And service life, there are more preferable toughness, abrasion resistance and high-temperature oxidation than non-coated tool, improve production efficiency.
Brief description
Fig. 1 is to compare in two kinds of coating cutting high hard material life-spans.
Specific embodiment
Embodiment 1
A kind of preparation method of the superhard gradient coating of tialsin of the present invention, comprises the following steps:
(1) surface of the work sandblasting and cleaning
Matrix is put in abrasive blast equipment, unlatching equipment carries out blasting treatment to surface of the work, remove surface oxide skin,
Dirt, erosion and its impurity.After sandblasting terminates, take out workpiece, recycle alcohol manually to carry out surface of the work cleaning, remove table
The residuals such as the greasy dirt in face.After manual cleaning finishes, workpiece is carried out clamping and sends in supersonic wave cleaning machine using super
Sound wave is cleaned automatically.After ultrasonic wave cleaning completes and dries workpiece, by clamping workpiece and send into warmed-up coating furnace chamber,
Startup program, after furnace chamber vacuumizes and substrate temperature reaches 400-500 DEG C, is passed through argon gas (ar), and flow is 180-
230sccm, setting bias is 700-950v, and vacuum is 0.005-0.008mbar, and workpiece is carried out with plasma cleaning, cleaning
Time is 15min.
(2) preparation of the superhard gradient coating of tialsin
The superhard gradient coating of tialsin, vacuum are coated with UHV condition using cathode ion coating technology to matrix
Room temperature controls at 400-500 DEG C, and holding vacuum is 0.005-0.06mbar, nitrogen (n2) flow be 150-220sccm, no
The corresponding target of coating phase together, bias voltage, target current are different.
A. the preparation of first stage ti prime coat layer.Continue to be passed through argon gas (ar) in vacuum furnace chamber, ar flow is 180-
230sccm, makes ti target be energized and is deposited, and electrical current is 120-150a, and bias voltage is 400-500v, and vacuum is
0.008mbar, sedimentation time is 30s-120s.
B. the preparation of second stage tin gradient coating.Stop being passed through ar, open n2Flow valve is passed through n into vacuum furnace chamber2,
n2Flow is 150-200sccm, and makes ti target continue to keep the "on" position in a, and electrical current is 120-150a, biased electrical
Press as 100-130v, vacuum is 0.007mbar, sedimentation time is 6-8min, obtains the tin coating that ti content is incremented by.
C. the preparation of phase III tial gradient coating.Stop being passed through n in vacuum furnace chamber2, it is passed through in furnace chamber simultaneously
Ar, ar flow is 180-230sccm, makes alti target and the energising of ti target, and alti target electrical current is 120-160a, ti target energising electricity
Flow for 120-150a, bias voltage is 100-120v, vacuum is 0.01-0.02mbar, sedimentation time is 20-30min, obtains
Gradient coating containing al.
D. the preparation of fourth stage tialn gradient coating.Contrary with step c, now stop being passed through ar in vacuum furnace chamber,
Continue to be passed through n in furnace chamber2, n2Flow is 180-200sccm, continues to make alti target and ti target be in "on" position, and alti target leads to
Electric current is 150-180a, and ti target electrical current is 120-150a, and bias voltage is 40-60v, and vacuum is 0.01-
0.02mbar, sedimentation time is 1.5h, obtains the tialn coating that al content is incremented by.
E. the preparation of the 5th stage tialsin gradient coating.Ti target power-off, continues to be passed through n in furnace chamber2, n2Flow is
180-250sccm, and continue to make alti target be in "on" position, electrical current is 150-180a, so that siti target is energized simultaneously, leads to
Electric current is 120-160a, and bias voltage is 60-80v, and vacuum is 0.04-0.06mbar, and sedimentation time is 42min.
F. the preparation of the 6th stage tisin gradient coating.Siti target continues to remain powered on state, remaining target power-off, leads to
Electric current is 140-160a, continues to be passed through n in furnace chamber2, n2Flow is 180-200sccm, and bias voltage is 60-80v, vacuum
Spend for 0.04-0.05mbar, sedimentation time is 20min.
(3) tialsin gradient coating is processed by shot blasting
Prepared on the matrix clamping having tialsin gradient coating and polishing machine, started polishing machine, and set polishing
Time and polishing velocity, start polishing program and are polished.
In technique scheme, it is that (purity is ti target for depositing target used by tialsin gradient coating
99.999%), alti target (wal:wti=70:30) and siti target (wsi:wti=20:80).
In technique scheme, the matrix after coating is processed by shot blasting, setting polishing time is 15min, polishing speed
Spend for 10m/s, not only can remove the drop of matrix surface after removing coating, surface can also be played with the effect of strengthening.
In technique scheme, the thickness of the tialsin gradient coating of preparation is 2.5-3.5 μm of one side, and elastic modelling quantity can
Reach 340gpa, high temperature oxidation resisting temperature is up to more than 1200 DEG C.In technique scheme, the tialsin gradient coating of preparation
Thickness is 2.5-3.5 μm of one side, and, up to 340gpa, high temperature oxidation resisting temperature is up to more than 1200 DEG C for elastic modelling quantity.
The high temperature resistant experiment of embodiment 2 tialsin
5 groups of high-speed steel (trade mark m2) sample of selection, every group 5 (every specification φ 20 × 5), by a mirror polish of sample,
Carry out tialsin coating according to process above, the one side thickness of coating is all 3 microns after whole sample cleaning.By prepare
Coating sample is respectively put in heating furnace by group, and the temperature setting heating furnace is 600 DEG C, 800 DEG C, 1000 DEG C, 1200 DEG C respectively
With 1400 DEG C, then with slow wire feeding, sample is cut, observes coating position section situation, result such as table 1 institute under ESEM
Show.
Table 1 high temperature tests scanning electron microscopic observation result
The high rigidity cutting experiment of embodiment 3 tialsin coating
Cutter: hard alloy bulb milling cutter, φ 10mm；
Machined material: Japanese Datong District mould steel dc53, hardness hrc60；
Cutting parameter: v=320m/min；
f=0.2mm/r；
ap=0.3mm；
vb=0.12mm；
The type of cooling: DRY CUTTING；
With reference to coating: Switzerland's commodity coating；
Select hard alloy bulb milling cutter in the present embodiment, high rigidity milling test is carried out by tialsin coating.At present
Market Shang Youyijia Switzerland Co., Ltd specialty is prepared milling cutter high rigidity and is cut coating, in order to compare, especially selects this Switzerland of family public
The coating that department produces is compared with tialsin coating.The coating that Switzerland Co., Ltd is produced is named as " Switzerland's commodity coating ".Real
Test result as shown in Figure 1.By experimental result as can be seen that tialsin coating is under identical experiment condition, milling matrix is hard
Spend the material for hrc60, milling length reaches 880 meters, and 430 meters of Switzerland's commodity coating milling of current commercialization.Real
Test result to show, the hard machining that the life-span in terms of hard machining for the tialsin coating has been significantly larger than commercialization on the market applies
Layer.
Claims (5)
1. a kind of preparation method of the superhard gradient coating of tialsin is it is characterised in that comprise the following steps:
1) step carrying out sandblasting to surface of the work, workpiece is put in abrasive blast equipment, and unlatching equipment enters to surface of the work
Row blasting treatment, removes oxide skin, dirt, erosion and its impurity on surface；
2) step that workpiece is carried out, workpiece after blasting treatment for the surface is carried out workpiece table first with alcohol
The cleaning in face, recycle ultrasonic wave surface of the work is carried out, finally again by plasma process to surface of the work at
Reason；
3) step that using cathode ion depositing process, workpiece is coated with the superhard gradient coating of tialsin, wherein, vacuum room temperature
Degree controls between 400-500 DEG C, and holding vacuum is 0.005-0.06mbar, and nitrogen flow is 150-220sccm, passes through
Six stages are coated with the superhard gradient coating of tialsin to workpiece, and the first stage prepares prime coat layer for ti, logical in vacuum furnace chamber
Enter argon gas, ar flow is 180-230sccm, so that ti target is energized and deposited, electrical current is 120-150a, bias voltage is
400-500v, vacuum is 0.008mbar, and sedimentation time is 30s-120s；Second stage is preparation tin gradient coating, stops
It is passed through ar, open n2Flow valve is passed through n into vacuum furnace chamber2, n2Flow is 150-200sccm, and makes ti target continue holding the
"on" position in one stage, electrical current is 120-150a, and bias voltage is 100-130v, and vacuum is 0.007mbar, sinks
The long-pending time is 6-8min, obtains the tin coating that ti content is incremented by；Phase III is preparation tial gradient coating, stops to vacuum
It is passed through n in furnace chamber2, it is passed through ar in furnace chamber, ar flow is 180-230sccm simultaneously, make alti target and the energising of ti target, alti target
Electrical current is 120-160a, and ti target electrical current is 120-150a, and bias voltage is 100-120v, and vacuum is 0.01-
0.02mbar, sedimentation time is 20-30min, obtains the gradient coating containing al；Fourth stage is preparation tialn gradient coating, stops
Only in vacuum furnace chamber, it is passed through ar, continue to be passed through n in furnace chamber2, n2Flow is 180-200sccm, continues to make alti target and ti target
It is in "on" position, alti target electrical current is 150-180a, ti target electrical current is 120-150a, bias voltage is 40-
60v, vacuum is 0.01-0.02mbar, and sedimentation time is 1.5h, obtains the tialn coating that al content is incremented by；5th stage was
Preparation tialsin gradient coating, ti target power-off, continues to be passed through n in furnace chamber2, n2Flow is 180-250sccm, and continues to make
Alti target is in "on" position, and electrical current is 150-180a, so that siti target is energized simultaneously, and electrical current is 120-160a, partially
Putting voltage is 60-80v, and vacuum is 0.04-0.06mbar, and sedimentation time is 42min；6th stage prepared gradient for tisin
Coating, siti target continues to remain powered on state, ti target and alti target power-off, and electrical current is 140-160a, continues in furnace chamber
It is passed through n2, n2Flow is 180-200sccm, and bias voltage is 60-80v, and vacuum is 0.04-0.05mbar, and sedimentation time is
20min；
4) step that tialsin gradient coating is processed by shot blasting, has been prepared the workpiece having tialsin gradient coating
On clamping and polishing machine, start polishing machine, and set polishing time and polishing velocity, start polishing program and be polished.
2. as claimed in claim 1, a kind of preparation method of the superhard gradient coating of tialsin it is characterised in that: for depositing
In target used by tialsin gradient coating, the purity of ti target is 99.999%, the mass ratio of al and ti is 70:30 in alti target,
In siti target, the mass ratio of si and ti is 20:80.
3. as claimed in claim 1, a kind of preparation method of the superhard gradient coating of tialsin it is characterised in that: setting polishing
Time is 10 ~ 20min, and polishing velocity is 8 ~ 15m/s.
4. as claimed in claim 1, a kind of preparation method of the superhard gradient coating of tialsin it is characterised in that: described
The thickness of tialsin gradient coating is 2.5-3.5 μm of one side.
5. as claimed in claim 1, a kind of preparation method of the superhard gradient coating of tialsin it is characterised in that: right at one
In the step that workpiece is carried out, during surface of the work being processed by plasma process, by clamping workpiece simultaneously
Send into warmed-up coating furnace chamber, startup program, after furnace chamber vacuumizes and when workpiece temperature reaches 400-500 DEG C, be passed through argon
Gas, flow is 180-230sccm, and setting bias is 700-950v, and vacuum is 0.005-0.008mbar, workpiece is carried out etc.
Ion Cleaning, scavenging period is 10 ~ 30min.
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