Ion source enhanced AlCrSiN coating with gradient Si content and gradient grain size
10941479 ยท 2021-03-09
Assignee
- ANHUI DUOJINTUCENG TECHNOLOGY CO. LTD. (Maanshan, CN)
- ANHUI HUALING AUTOMOBILE CO., LTD. (Maanshan, CN)
- ANHUI UNIVERISTY OF TECHNOLOGY (Maanshan, CN)
Inventors
- Shihong ZHANG (Maanshan, CN)
- Fei Cai (Maanshan, CN)
- Qimin Wang (Maanshan, CN)
- Lin Zhang (Maanshan, CN)
- Biao Wang (Maanshan, CN)
- Lu Wang (Maanshan, CN)
- Ying Gao (Maanshan, CN)
- Wei Fang (Maanshan, CN)
- Jiagang Liang (Maanshan, CN)
Cpc classification
C23C28/048
CHEMISTRY; METALLURGY
C23C14/022
CHEMISTRY; METALLURGY
C23C28/044
CHEMISTRY; METALLURGY
C23C28/042
CHEMISTRY; METALLURGY
International classification
C23C14/00
CHEMISTRY; METALLURGY
Abstract
An ion source enhanced AlCrSiN coating for a cutting tool is provided. The ion source enhanced AlCrSiN coaling has gradient Si content and grain size, including sequentially an AlCrSiN working layer, an interlayer and an AlCrN bottom layer in order from a surface of the coating to a substrate, wherein from the AlCrN bottom layer to the AlCrSiN working layer, Si content in the interlayer is gradually increased, and the interlayer has a texture that changes from coarse columnar crystals to fine nanocrystals and amorphous body. A texture of the coating, in which the grain size is gradually decreased, sequentially includes coarse columnar crystals, fine columnar crystals and fine equiaxed crystals. A method for preparing the ion source enhanced AlCrSiN coating with the gradient Si content and grain size is provided as well as a cutting tool having the coating deposited thereon.
Claims
1. An ion source enhanced AlCrSiN coating with a gradient Si content and a gradient grain size, comprising sequentially an AlCrSiN working layer, an interlayer and an AlCrN bottom layer in order from a surface of the ion source enhanced AlCrSiN coating to a substrate, wherein from the AlCrN bottom layer to the AlCrSiN working layer, the Si content in the interlayer is gradually increased, and the interlayer comprises a texture changing from coarse columnar crystals to fine nanocrystals and amorphous body, the texture sequentially comprises coarse columnar crystals, fine columnar crystals and fine equiaxed crystals, the grain size of the interlayer is gradually decreased, in the interlayer, the Si content is gradually increased from 1 wt. % to 5 wt. %, and the grain size is gradually decreased from 60 nm to 20 nm.
2. The ion source enhanced AlCrSiN coating with the gradient Si content and the gradient grain size according to claim 1, wherein Cr in the ion source enhanced AlCrSiN coating is completely or partially replaced by Ti to obtain an AlTiSiN coating or an AlCrTiSiN coating.
3. The ion source enhanced AlCrSiN coating with the gradient Si content and the gradient grain size according to claim 1, wherein the substrate is subjected to an etching and cleaning in advance, comprising the steps of: evacuating a vacuum oven for a multi-arc ion plating to 2.010.sup.4 Pa, and then introducing Ar gas to the vacuum oven to adjust a pressure of the vacuum oven to 4.0 Pa and heating the vacuum oven to 450 C., turning on a cleaning Ti target, and then turning on an anode target, so as to form positive and negative electrodes with the cleaning Ti target to achieve a traction of electron motion, allowing electrons to collide with the Ar gas to generate Ar.sup.+, and then controlling a negative bias voltage to 200 V, thereby attracting the Ar.sup.+ to perform an ion bombardment on a surface of the substrate for a bombardment time of 45 min.
4. The ion source enhanced AlCrSiN coating with the gradient Si content and the gradient grain size according to claim 1, wherein the ion source enhanced AlCrSiN coating has a coefficient of friction of 0.36-0.40 at room temperature.
5. The ion source enhanced AlCrSiN coating with the gradient Si content and the grain size according to claim 1, wherein the ion source enhanced AlCrSiN coating has a microhardness greater than 3800 HK.
6. A method for preparing the ion source enhanced AlCrSiN coating with the gradient Si content and the gradient grain size according to claim 1, wherein the AlCrSiN coating is deposited by the steps of: (1) evacuating a vacuum oven to a background vacuum of 110.sup.4 to 210.sup.4 Pa, and raising a temperature of the vacuum oven to 480 C.; (2) introducing Ar gas to the vacuum oven, controlling a vacuum degree in the vacuum oven to 4.0 Pa and controlling a negative bias voltage for the substrate to 200 V, and then turning on a Ti target and controlling a target current of the Ti target to 80 A, followed by performing an etching and cleaning on a surface of the substrate by a high-energy ion bombardment at the negative bias voltage for the substrate of 200 V for a cleaning time of 45 min; (3) turning off the Ti target and introducing nitrogen gas to the vacuum oven, controlling the negative bias voltage for the substrate to 60 V and adjusting the vacuum degree in the vacuum oven to 3.5 Pa, the nitrogen gas being introduced in such way to maintain a constant pressure at the vacuum degree of 3.5 Pa, using two sets of AlCr targets, and adjusting currents of the two sets of the AlCr targets to 130 A for a period of 77 min; (4) continuously operating the two sets of the AlCr targets with the preset parameters, and adjusting a target current of an AlCrSi target to 130 A with the negative bias voltage for the substrate still being 60 V for a period of 58 min; (5) turning off one set of the AlCr targets, and continuously operating the remaining AlCr targets and the AlCrSi target with the preset parameters for a period of 88 min; and (6) turning off the two sets of the AlCr targets, and continuously operating the AlCrSi target with the preset parameters for a period of 120 min.
7. The method according to claim 6, wherein each AlCr target of the two sets of the AlCr targets has an atomic ratio of Al to Cr of 70:30.
8. The method according to claim 6, wherein the AlCrSi target has an atomic ratio of Al:Cr:Si of 60:30:10.
9. A cutting tool comprising the ion source enhanced AlCrSiN coating according to claim 1.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION OF THE EMBODIMENTS
(26) Hereinafter, embodiments of the present invention will be described in detail. The embodiments are implemented based on the technical solutions of the present invention and the detailed implementations and specific operating procedures are provided. However, the protection scope of the present invention is not limited by the following embodiments.
Embodiment 1
(27) As shown in
(28) A pre-treated high-speed steel cutting tool was evenly fixed on a rotating stand in the chamber, and the rotation speed of the rotating stand was controlled to 3 rpm. After that, the chamber was evacuated to a background vacuum of 110.sup.4 to 210.sup.4 Pa, while turning on a heater to raise the temperature to 480 C.
(29) When the vacuum degree in the vacuum oven reached 2.010.sup.4 Pa, Ar gas with a purity of 99.999% was introduced, followed by heating to 450 C. The cylindrical Ti target was turned on as a traction arc target. The current during cleaning was controlled to 40 A, so that a large number of electrons were excited. A circular auxiliary anode target was turned on to form a positive electrode and a negative electrode with the Ti target, thereby achieving traction of electron motion. The electrons collided with the Ar gas in the vacuum oven to generate high density of Ar.sup.+. Negative bias voltage for the substrate was set to 200 V, attracting the Ar.sup.+ to perform ion bombardment on the surface of the substrate for the bombardment time of 45 min.
(30) After that, the cylindrical Ti arc target was turned off, and a N.sub.2 flow valve was opened, followed by controlling the negative bias voltage for the substrate to 60 V and adjusting the vacuum degree in the vacuum oven to about 3.5 Pa. N.sub.2 was introduced in such way to maintain a constant pressure. Two sets of AlCr targets were used and their currents were adjusted to 130 A for a period of 252 min.
(31) Then, the AlCr targets were turned off, and the current of a set of AlCrSi targets was adjusted to 130 A, with the negative bias voltage for the substrate still being 60 V, for a period of 122 min. Finally, the AlCrSi targets were turned off, the bias voltage power supply was turned off and the N.sub.2 flow valve was closed to complete the coating process. The cutting tool was cooled along with the vacuum oven to 25 C. and then removed.
(32) The substrate which was subjected to the ion etching and cleaning, and the prepared coating were tested.
Embodiment 2
(33) In the present embodiment, the current for cleaning of the Ti cylindrical arc was controlled to 70 A during the process of the high-energy Ar.sup.+ ion etching. The substrate which was subjected to the ion etching and cleaning, and the prepared coating were tested.
(34) For other aspects, this embodiment was performed in the same manner as in Embodiment 1.
Embodiment 3
(35) In the present embodiment, the current for cleaning of the Ti cylindrical arc was controlled to 100 A during the process of the high-energy Ar.sup.+ ion etching. The substrate which was subjected to the ion etching and cleaning, and the prepared coating were tested.
(36) For other aspects, this embodiment was performed in the same manner as in Embodiment 1. The AlCrSiN coating prepared in this embodiment was denoted as AlCrSiN-1, and the coating included sequentially an AlCrSiN working layer and an AlCrN bottom layer in order from the surface of the coating to the substrate.
(37) The detailed process parameters for the cleaning and deposition of the coating in each of the above embodiments are shown in Table 1.
(38) TABLE-US-00001 TABLE 1 Detailed process parameters for cleaning and deposition of AlCrSiN coatings. substrate bias gas flow substrate voltage (ml/min) target current (A) temperature deposition step (V) Ar N.sub.2 Ti AlCr AlCrSi ( C.) time (min) 1 200 650 0 40 0 0 450 70 100 2 60 0 680 0 130 0 450 252 3 60 0 680 0 0 130 450 122
(39) The sample of each embodiment, after being prepared, was subjected to relevant tests. The test results of the AlCrSiN coatings are shown in Table 2.
(40) TABLE-US-00002 TABLE 2 Test results of AlCrSiN coatings. L.sub.c2 surface roughness coating (N) HF R.sub.a S.sub.q I.sub.40 41 HF3 140 226 I.sub.70 46 HF2 88 140 I.sub.100 52 HF1 69 117
(41) In order to compare the three cleaned substrates and coatings in Embodiment 1, Embodiment 2 and Embodiment 3, the following tests were performed.
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Embodiment 4
(45) In the present embodiment, an AlCrSiN composite coating for cutting tools was specifically prepared by the following method.
(46) A pre-treated high-speed steel cutting tool was evenly fixed on a rotating stand in the chamber, and the rotation speed of the rotating stand was controlled to 3 rpm. After that, the chamber was evacuated to a background vacuum of 110.sup.4 to 2.sup.4 Pa, while turning on a heater to raise the temperature to 480 C.
(47) When the vacuum degree in the vacuum oven reached 2.010.sup.4 Pa, Ar gas with a purity of 99.999% was introduced, followed by heating to 450 C. The cylindrical Ti target was turned on as a traction arc target. The current during cleaning was controlled to 100 A, so that a large number of electrons were excited. A circular auxiliary anode target was turned on to form a positive electrode and a negative electrode with the Ti target, thereby achieving traction of electron motion. The electrons collided with the Ar gas in the vacuum oven to generate Ar.sup.+ having high density. Negative bias voltage for the substrate was set to 200 V, attracting the Ar.sup.+ to perform ion bombardment on the surface of the substrate for a bombardment time of 45 min.
(48) After that, the cylindrical Ti target was turned off, and a N.sub.2 flow valve was opened, followed by controlling the negative bias voltage for the substrate to 6 V and adjusting the vacuum degree in the vacuum oven to about 3.5 Pa. N.sub.2 was introduced in such way to maintain a constant pressure. Two sets of AlCr targets were used and their currents were adjusted to 130 A for a period of 77 min.
(49) Then, the two sets of AlCr targets were continued to operate with the preset parameters, and the current of a set of AlCrSi targets was adjusted to 130 A, with the negative bias voltage for the substrate still being 60 V, for a period of 58 min.
(50) Afterward, one set of the AlCr targets were turned off, and the remaining AlCr targets and the AlCrSi targets were continued to operate with the preset parameters for a period of 88 min.
(51) Then, the AlCr targets were turned off, and the set of the AlCrSi targets were continued to operate with the preset parameters for a period of 120 min. Finally, the AlCrSi targets were turned off, the bias voltage power supply was turned off and the N.sub.2 flow valve was closed to complete the coating process. The cutting tool was cooled along with the oven to 25 C. and removed.
(52) As shown in
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(55) The coating had a surface microhardness of 3813.4 HK. The coating had a coefficient of friction of 0.36 to 0.4 in a ball-on-disc friction and wear test. The coatings were deposited on high-speed steel vertical milling cutters to perform cutting test for comparison under the following cutting conditions: wet cutting (water-based cutting fluid, the ratio of cutting fluid to water of 1:30); material to be cut: 20 CrMo (normalized, HB200); cutting speed: 94.2 m/min; feedrate: 600 mm/min; and axial and radial depth of cut: 2 mm. Even in such harsh environments, the service life of the coated cutting tool was increased by 2 times or more.
(56) To compare the two coatings of Embodiment 3 and Embodiment 4, the following tests were performed.
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Embodiment 5
(59) In this embodiment, an AlTiSiN coating, in which Cr in the AlCrSiN composite coating for cutting tools was completely replaced by Ti, was specifically prepared by the following method.
(60) A pre-treated high-speed steel cutting tool was evenly fixed on a rotating stand in the chamber, and the rotation speed of the rotating stand was controlled to 3 rpm. After that, the chamber was evacuated to a background vacuum of 110.sup.4 to 210.sup.4 Pa, while turning on a heater to raise the temperature to 480 C.
(61) When the vacuum degree in the vacuum oven reached 2.010.sup.4 Pa, Ar gas with a purity of 99.999% was introduced, followed by heating to 450 C. The cylindrical Ti target was turned on as a traction arc target. The current during cleaning was controlled to 100 A, so that a large number of electrons were excited. A circular auxiliary anode target was turned on to form a positive electrode and a negative electrode with the Ti target, thereby achieving traction of electron motion. The electrons collided with the Ar gas in the vacuum oven to generate Ar.sup.+ having high density. Negative bias voltage for the substrate was set to 200 V, attracting the Ar.sup.+ to perform ion bombardment on the surface of the substrate for a bombardment time of 45 min.
(62) After that, the cylindrical Ti target was turned off, and a N.sub.2 flow valve was opened, followed by controlling the negative bias voltage for the substrate to 60 V and adjusting the vacuum degree in the vacuum oven to about 3.5 Pa. N.sub.2 was introduced in such way to maintain a constant pressure. Two sets of AlTi targets (Al:Ti=67:33) were used and their currents were adjusted to 120 A for a period of 75 min.
(63) Then, the two sets of AlTi targets were continued to operate with the preset parameters, and the current of a set of AlTiSi targets (Al:Ti:Si=60:30:10) was adjusted to 120 A, with the negative bias voltage for the substrate still being 60 V, for a period of 55 min.
(64) Afterward, one set of the AlTi targets were turned off, and the remaining AlTi targets and the AlTiSi targets were continued to operate with the preset parameters for a period of 85 min.
(65) Then, the AlTi targets were turned off, and the set of the AlTiSi targets were continued to operate with the preset parameters for a period of 120 min. Finally, the AlTiSi targets were turned off, the bias voltage power supply was turned off and the N.sub.2 flow valve was closed to complete the coating process. The cutting tool was cooled along with the oven to 25 C. and then removed.
Embodiment 6
(66) In this embodiment, an AlCrTiSiN coating, in which Cr in the AlCrSiN composite coating for cutting tools was partially replaced by Ti, was specifically prepared by the following method.
(67) A pre-treated high-speed steel cutting tool was evenly fixed on a rotating stand in the chamber, and the rotation speed of the rotating stand was controlled to 3 rpm. After that, the chamber was evacuated to a background vacuum of 110.sup.4 to 210.sup.4 Pa, while turning on a heater to raise the temperature to 480 C.
(68) When the vacuum degree in the vacuum oven reached 2.010.sup.4 Pa, Ar gas with a purity of 99.999% was introduced, followed by heating to 450 C. The cylindrical Ti target us turned on as a traction arc target. The current during cleaning was controlled to 100 A, so that a large number of electrons were excited. A circular auxiliary anode target was turned on to form a positive electrode and a negative electrode with the Ti target, thereby achieving traction of electron motion. The electrons collided with the Ar gas in the vacuum oven to generate Ar.sup.+ having high density. Negative bias voltage for the substrate was set to 200 V, attracting the Ar.sup.+ to perform ion bombardment on the surface of the substrate for a bombardment time of 45 min.
(69) After that, the cylindrical Ti target was turned off, and a N.sub.2 flow valve was opened, followed by controlling the negative bias voltage for the substrate to 60 V and adjusting the vacuum degree in the vacuum oven to about 3.5 Pa. N.sub.2 was introduced in such way to maintain a constant pressure. Two sets of AlCr targets (Al:Cr=70:30) were used and their currents were adjusted to 130 A for a period of 75 min.
(70) Then, the two sets of AlCr targets were continued to operate with the preset parameters, and the current of a set of AlTiSi targets (Al:Ti:Si=60:30:10) was adjusted to 120 A, with the negative bias voltage for the substrate still being 60 V, for a period of 55 min.
(71) Afterward, one set of the AlCr targets were turned off, and the remaining AlTi targets and the AlTiSi targets were continued to operate with the preset parameters for a period of 200 min.
(72) Finally, the AlTi targets and the set of the AlTiSi targets were turned off, the bias voltage power supply was turned off and the N.sub.2 flow valve was closed to complete the coating process. The cutting tool was cooled along with the oven to 25 C.; and removed.
(73) The above descriptions are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention shall fall within the protection scope of the claims of the invention.