CN106148894B - A kind of W-B-C hard coat and its preparation method and application - Google Patents
A kind of W-B-C hard coat and its preparation method and application Download PDFInfo
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- CN106148894B CN106148894B CN201510185874.3A CN201510185874A CN106148894B CN 106148894 B CN106148894 B CN 106148894B CN 201510185874 A CN201510185874 A CN 201510185874A CN 106148894 B CN106148894 B CN 106148894B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 15
- 238000000151 deposition Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000004544 sputter deposition Methods 0.000 claims abstract description 7
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 229910016459 AlB2 Inorganic materials 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 4
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 claims description 3
- 238000005137 deposition process Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
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- 239000000203 mixture Substances 0.000 description 5
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
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- 238000001228 spectrum Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
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- 239000002245 particle Substances 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- 230000001050 lubricating effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
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Abstract
The invention discloses a kind of W-B-C hard coats and its preparation method and application, belong to metal material surface deposition hard wear-resistant coating technical field.Using the method for magnetically controlled DC sputtering, by regulating and controlling C2H2Partial pressure, depositing temperature and substrate bias, are prepared for W-B-C hard wear-resistant coating on hard alloy substrate.Higher microhardness, lower average friction coefficient and wear rate is presented in the structure coating.This W-B-C (AlB according to the present invention2Type) hard coat is successfully synthesized, can significantly improve the hardness and wearability of cutter or workpiece surface, be of great significance for the theoretical research and practical application of superhard boride coating.
Description
Technical field:
The invention belongs to metal material surfaces to deposit hard wear-resistant coating technical field, and specifically a kind of W-B-C is hard
Matter coating and its preparation method and application.
Background technique:
Superhard material is widely used in the fields such as machining industry, mould industry, geological drilling and aerospace.But
With the fast development of modern industry, difficult-to-machine material is more and more so that certain conventional tool materials be unable to satisfy it is increasingly multiple
Miscellaneous cutting ability requirement.Therefore, find that novel high hardness material is laboratory staff and what theoreticians were concerned about very much grinds
Study carefully project.
AlB in recent years2-type WB2It is considered as a kind of super-hard self-lubricating film of great potential, has become calculating
With the research hotspot of experimental field.Woods in 1966 et al. prepares AlB using hot-wire chemical gas-phase deposition for the first time2-type
WB2, some researchers attempt to prepare the phase, but fall throughs using powder metallurgic method later, because theoretical calculation shows
AlB2-type WB2It is a kind of high pressure phase.Until 2013, Jiang etc. was prepared by the method for magnetically controlled DC sputtering at 680 DEG C
Smooth fine and close, high rigidity low abrasion AlB out2-type WB2Film, and its relevant physical property and growth mechanism are carried out
Research.But the depositing temperature of Jiang is excessively high, is difficult to promote in the industry, while it is to WB2The structure of base film and
Performance is studied and is improved.The research of transition metal boride at present focuses mostly in terms of high temperature and pressure block synthesis, and has
The research for closing films/coatings preparation aspect is less.Therefore, high performance W-B-C film is prepared by doping appropriate, it can be significant
The hardness and wearability for improving cutter or workpiece surface, theoretical research and practical application for superhard boride coating have weight
Want meaning.
Summary of the invention
The purpose of the present invention is to provide a kind of W-B-C (AlB2Type) hard coat and its preparation method and application, the painting
Layer can be improved cutter or workpiece surface hardness and wearability.
The technical scheme is that
A kind of preparation method of W-B-C hard coat, the W-B-C hard coat are with AlB2The C of structure adulterates WB2
Film, C doping are 26.4-72.5at.%；The hard coat selects WB2Type WB2Target, simultaneously using magnetically controlled DC sputtering technology
By controlling C2H2Partial pressure, depositing temperature and substrate bias are prepared on the substrates such as hard alloy.
Using the corresponding target of ingredient metering ratio, guarantees target material composition B/W (at.%=2), accurately control C2H2Gas point
The technological parameters such as pressure, depositing temperature and substrate bias, conducive to effective control of coating composition and structure.
The W-B-C hard coat is prepared using magnetically controlled DC sputtering technology to include the following steps:
(1) it is put into after being pre-processed to substrate in the vacuum chamber of magnetically controlled DC sputtering technical equipment, to true in vacuum chamber
Reciprocal of duty cycle reaches 5 × 10-3Pa~1 × 10-2When Pa, argon gas is then passed to, ar pressure is controlled in 0.5~2Pa, is then turned on matrix
It is biased into -100V~-300V, makes argon gas that glow discharge occur, aura is carried out to substrate and is cleaned 5~15 minutes；
(2) W-B-C hard coat: deposition process technological parameter is deposited are as follows: target-substrate distance is 50~100mm, C2H2Partial pressure
0.004-0.05Pa, 300~400V of target voltage, 0.5~1.5A of electric current, pulsed bias be -50~-300V, duty ratio 20~
40%, 100~600 DEG C of depositing temperature, coating layer thickness is 1~3 μm.
In above-mentioned steps (1), preprocessing process is carried out to substrate are as follows: substrate surface is polishing to Ra=0.4 μm, is then adopted
It is cleaned by ultrasonic 15min with acetone, then is dried after being rinsed with alcohol.
After above-mentioned steps (2) deposit, stopping is passed through C2H2With Ar gas, substrate bias is closed, shielding power supply is closed and opens
It closes, continues to vacuumize, until gained coating sample cools to 50 DEG C with the furnace hereinafter, taking out.
The present invention has the following advantages and beneficial effects:
1, the present invention is the W-B-C coating in carbide surface synthesis, and film hardness can reach 40GPa or more, film/base
Binding force reaches 50N or more and good friction and wear behavior, and (coefficient of friction~0.316, wear rate is down to 7.7 × 10- 8mm3/mN)。
2, present invention demonstrates that WB2High pressure phase and its a possibility that being synthesized, is entrained under the conditions of low-temp low-pressure.
3, W-B-C (AlB according to the present invention2Type) coating can be applied to the protection of cutter or workpiece surface, and can have
Effect prolongs its service life.
Detailed description of the invention:
Fig. 1 is different C2H2The X-ray diffraction spectrum of the lower W-B-C film prepared of partial pressure.
Fig. 2 is different C2H2The section SEM and surface A FM shape appearance figure of the lower W-B-C film prepared of partial pressure.
Fig. 3 is different C2H2The hardness H and effective modulus of elasticity E* of the lower W-B-C film prepared of partial pressure.
Fig. 4 is different C2H2The coefficient of friction of the lower W-B-C film prepared of partial pressure and abrasion.
Specific embodiment:
The present invention is described in further details below by example.
Embodiment 1
Substrate uses YG8 hard alloy.After plated film front surface first passes through grinding, polishing, ultrasonic cleaning, drying, it is put into true
On empty room sample stage, reach 5 × 10 to vacuum degree in vacuum chamber-3When Pa, gas mass flow controller is opened, logical argon gas arrives
2.0Pa, matrix add DC negative bias voltage to -180V, carry out aura to sample and clean 15 minutes.Hereafter, into film deposition process,
Specific process parameter are as follows: target-substrate distance 50mm, C2H2Partial pressure (PC2H2) respectively select 0Pa, 0.004Pa, 0.006Pa,
0.008Pa, 0.01Pa, 0.02Pa, 0.03Pa, 0.04Pa, 0.05Pa set C2H2Total gas pressure with argon gas is 0.5Pa, target electricity
0.5A is flowed, pulsed bias is -50V, and duty ratio 30%, 400 DEG C of depositing temperature, total sedimentation time is 90 minutes.After deposition,
Gas flow, which is passed through, to be automatically closed, and drop bias, closing target power supply switch stop the supple of gas or steam, continue to vacuumize, furnace cooling rapidly at this time
When being down to 50 DEG C or less to vacuum room temperature, finally bleeds off vacuum and take out workpiece.
The XRD spectrum of coating is as shown in Figure 1, it can be seen from the figure that C2H2The size of partial pressure can change film significantly
Phase structure.Pure WB2Film shows the growth of (101) preferred orientation；Work as C2H2When partial pressure increases to 0.008Pa from 0.004Pa,
The preferred orientation of film is changed into (001) by (101)；And work as PC2H2Only occur when=0.01Pa, in the diffracting spectrum of film non-
Normal faint and wideization (001) diffraction maximum；With C2H2Partial pressure further increases, WB in film2The diffraction maximum of phase all disappears
Mistake instead XRD non crystalline structure.According to XRD data, with C2H2The lattice constant of the increase of partial pressure, film gradually becomes
Greatly, this illustrates that lesser C atom tendency gap is solid-solution in h-WB2Interstitial solid solution is formed in lattice.It can also be sent out from Fig. 1
It is existing, as 0.004Pa≤PC2H2When≤0.008Pa, the crystallinity of W-B-C film is higher than pure WB2Film.In addition, for crystallization
W-B-C film, with C2H2The increase of partial pressure, (001) diffraction maximum of film gradually wideization, shows the crystallite dimension of film gradually
It reduces, one side C can promote second nucleation, and growing up for crystal grain can be prevented by being on the other hand gathered in the C near crystal boundary.Separately
Outside, the generation of other phases, such as WC are not found in the XRD diffracting spectrum of all samples.
Fig. 2 gives four typical difference C2H2The section SEM and surface A FM shape of the lower W-B-C film prepared of partial pressure
Looks figure.It can be obtained from the figure that pure WB2Film (PC2H2=0Pa) section shows typical column structure；Work as PC2H2=0.006Pa
When, the pillar cell size of film reduces and is changed into thinner fibrous structure；With in film, C content is further increased
(PC2H2=0.01Pa), the microstructure of film is changed into fine and close undefined structure, and sample is mainly by h-WB at this timexCy/a-
WC/a-C composition；Work as C2H2When partial pressure increases to 0.03Pa, film sections show glassy pattern, and film is mainly by one at this time
A little spherical or sheet unordered a-C compositions.As C content increases in film, this differentiation of film sections pattern also exists
It is observed in WC/a-C nano compound film.It can be seen that from the surface A FM shape appearance figure of film in PC2H2=0,0.006Pa
The fusiform particle that observed nano-scale in the film of lower preparation, show the anisotropic growth of film, in addition film
Cluster size is with C2H2The increase of partial pressure and significantly reduce it is consistent with the variation tendency of Cross Section Morphology, this be primarily due to C original
The addition of son can refine crystal grain, while also make the structure of film more and more finer and close；Work as PC2H2When=0.01Pa, nothing is presented in film
The surface topography of sizing；PC2H2There is the cluster particle of sheet in=0.03Pa, film surface, these particles may be a-C.
Fig. 3 is different C2H2The hardness H and effective modulus of elasticity E* of the lower W-B-C film prepared of partial pressure.Found out by figure, with
C2H2Partial pressure increases, and the hardness H of film shows the trend for first increasing and reducing afterwards, and in PC2H2When=0.006,0.008Pa,
The hardness highest (45GPa or so) of film, than pure WB2Film hardness is higher by about 10GPa, has reached wanting for superhard thin film
It asks.The reason of micro C doping causes film hardness to be significantly increased can be several from film microstructure, phase composition and stress intensity etc.
A angle is explained, after mixing C: (1) film crystal grain refinement, and crystallinity increases, and structure is finer and close, increase film hardness；(2)
Film compression increases, conducive to the promotion of film hardness；(3) preferred orientation of film is changed into (001) from (101), in solid matter
In hexagonal structure, the film hardness with higher of (001) orientation；(4) solid solution strengthening effect of C atom increases film hardness
Add；(5) work as PC2H2When=0.006,0.008Pa, the phase composition of film is mainly h-WBxCy/ a-WC or (and) h-WBxCy/a-
WC/a-C, crystallite dimension are about 5~6nm, crystalline phase by relatively thin amorphous phase a-WC or (and) a-C coats, this compound
Structure can make the formation of film Dislocations and the relaxation of discontinuous stress be inhibited, so as to cause film hardness increasing
Add.Work as PC2H2When >=0.01Pa, the hardness of film is gradually decreased, this amorphous phase being primarily due in film (a-WC, a-C) contains
It measures more and more.In addition, the effective modulus of elasticity E* of film is with PC2H2Increase and is gradually reduced and the changing rule of hardness H
It is not consistent.
Fig. 4 is different C2H2The coefficient of friction and wear rate of the lower W-B-C film prepared of partial pressure.As can be seen from Fig., with
C2H2Partial pressure increases, and broken line variation is presented in the coefficient of friction and wear rate of film.(1) as 0Pa≤PC2H2When≤0.008Pa, with
C2H2Partial pressure increases, and the coefficient of friction and wear rate of film gradually decrease, and in PC2H2Reach minimum value when=0.008Pa, wherein
Coefficient of friction is 0.316, and wear rate is down to 7.7 × 10-8mm3/mN.(2) work as PC2H2When=0.01Pa, the coefficient of friction of film drops
Down to 0.27, wear rate is also relatively low, is 9.2 × 10-8mm3/ mN, it is h-WB that low wear rate, which is primarily due to this film,xCy/
A-WC/a-C nano composite structure, and there is certain hardness (31.3GPa), minimum surface roughness, suitable compression,
Most importantly there is a certain amount of a-C to generate, make in wear process that there are lubricating actions.(3) work as PC2H2It is thin when=0.02Pa
The coefficient of friction and wear rate of film sharply increase, and wear rate is up to 1.98 × 10-6mm3/ mN, although having had in film more
A-C is generated, but since film residual compression is excessive, film in wear process is made to be easy to crack and unstable wear；(4) when
PC2H2When=0.03Pa, the coefficient of friction and wear rate of film decrease, although its hardness is only 3.9GPa, its wear rate
Have been lowered to 4.57 × 10-7mm3/ mN, and coefficient of friction is only 0.106.This self-lubricating property for being primarily due to this film increases
By force, and there is suitable compression.(5) work as PC2H2When >=0.04Pa, the coefficient of friction of film is lower, but wear rate is anxious
Increase severely and add, this is primarily due to, and film hardness is too low (< 1GPa), and film does not have good support and makees under plus load effect
With and make abrasion aggravate.
Embodiment the result shows that, the present invention is successfully prepared W-B-C under non-equilibrium condition by magnetron sputtering technique
(AlB2Type) coating, which presents high rigidity and excellent friction and wear behavior, can significantly improve cutter or workpiece surface
Hardness and wearability, be of great significance for the theoretical research and practical application of superhard boride coating.
Claims (4)
1. a kind of preparation method of W-B-C hard coat, it is characterised in that: the W-B-C hard coat is with AlB2Structure
C adulterates WB2Film, C doping are 26.4-72.5at.%；The hard coat selects WB2Type WB2Target is splashed using direct magnetic control
Penetrate technology and by control C2H2Partial pressure, depositing temperature and substrate bias, are prepared on cemented carbide base material；It is described
WB2In the chemical component of target, the ratio of the atomic percentage content of B and W is 2；Using described in the preparation of magnetically controlled DC sputtering technology
W-B-C hard coat includes the following steps:
(1) it is put into after being pre-processed to substrate in the vacuum chamber of magnetically controlled DC sputtering technical equipment, to vacuum degree in vacuum chamber
Reach 5 × 10-3Pa~1 × 10-2When Pa, argon gas is then passed to, ar pressure is controlled in 0.5~2Pa, is then turned on substrate bias
To -100V~-300V, make argon gas that glow discharge occur, aura is carried out to substrate and is cleaned 5~15 minutes；
(2) W-B-C hard coat: deposition process technological parameter is deposited are as follows: target-substrate distance is 50~100mm, C2H2With total gas of argon gas
Pressure is 0.5Pa, C2H2Divide 0.004-0.05Pa, 300~400V of target voltage, 0.5~1.5A of electric current, pulsed bias be -50~-
300V, duty ratio 20~40%, 100~600 DEG C of depositing temperature, coating layer thickness is 1~3.0 μm；After deposition, stop being passed through
C2H2With Ar gas, substrate bias is closed, shielding power supply switch is closed, continues to vacuumize, until the furnace cooling of gained coating sample
To 50 DEG C hereinafter, taking out.
2. the preparation method of W-B-C hard coat according to claim 1, it is characterised in that: step (1) carries out substrate
Preprocessing process are as follows: substrate surface is polishing to Ra=0.4 μm, 15min is then cleaned by ultrasonic using acetone, then rinsed with alcohol
After dry.
3. a kind of W-B-C hard coat prepared using claim 1 the method, it is characterised in that: the hard coating film
Hardness can reach 40GPa or more, and film/base junction resultant force reaches 50N or more, and coefficient of friction is lower than 0.316, wear rate down to 7.7 ×
10-8mm3/mN。
4. the application of W-B-C hard coat according to claim 3, it is characterised in that: the hard coat is applied to cutter
Or the protection of workpiece surface.
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| CN115181948A (en) * | 2022-07-06 | 2022-10-14 | 中国科学院金属研究所 | W-Si-B hard coating and preparation method and application thereof |
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