CN102061454A - Method for preparing coating on cutter - Google Patents
Method for preparing coating on cutter Download PDFInfo
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- CN102061454A CN102061454A CN 201110024134 CN201110024134A CN102061454A CN 102061454 A CN102061454 A CN 102061454A CN 201110024134 CN201110024134 CN 201110024134 CN 201110024134 A CN201110024134 A CN 201110024134A CN 102061454 A CN102061454 A CN 102061454A
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Abstract
The invention provides a method for preparing a coating on a cutter, relating to a cutter. The method comprises the following steps of: putting a numeric control cutter blade in a reaction chamber, vacuumizing the reaction chamber, introducing a gas mixture of TiCl4, N2 and H2, and depositing a TiN layer on the surface of the cutter; introducing a gas mixture of TiCl4, N2, CH3CN and H2, and depositing an MT-TiCN layer on the surface of the TiN layer; closing a gas source, introducing a gas mixture of TiCl4, AlCl3, CO, CO2, CH4, N2 and H2, and depositing a binding-phase AlTiCNO layer; in the gas mixture of TiCl4, CO, CO2, CH4, N2 and H2, depositing a TiCO layer; in a gas mixture of CO2, AlCl3, HCl and H2, depositing an aluminum oxide nucleating layer; and introducing a gas mixture of AlCl3, CO, CO2, HCl, H2S and H2, and depositing an aluminum oxide coating. The coating has high surface finish quality and finer and uniform grains.
Description
Technical field
The present invention relates to a kind of cutter, especially relate to a kind of on cutter the preparation method of applying coating.
Background technology
It in cutting tool surface-coated coating one of important channel of improving the cutting tool performance, coated cutting tool has that surface hardness height, wear resistance are good, stable chemical performance, heat-resistant oxidized, characteristics such as frictional coefficient is little and thermal conductivity is low, and comparable not coated cutting tool improves the life-span more than 5～10 times during cutting.The high-quality process for modifying surface that the top coat technology of cutting tool grows up as the market requirement, because this technology can make cutting tool obtain good comprehensive mechanical performance, not only can improve cutting tool work-ing life effectively, and can also improve mechanical workout efficient significantly, so this technology becomes one of gordian technique of cutting tool manufacturing.
Al
2O
3Coating has very high chemical stability and good thermal barrier characteristics, is high speed cutting tool ideal coated material.In addition, it is emphasized that CVD remains can the high-quality Al of economic production at present
2O
3The unique technical means of coating.Can pass through CVD process deposits Al
2O
3Coating can obtain three kinds of different phases, is respectively α-Al
2O
3, k-Al
2O
3And γ-Al
2O
3, α-Al wherein
2O
3Be unique stable Al
2O
3Phase.Metastable κ mutually mutually will be by being converted into stable α phase as the heat that produces in thermal treatment, post-depositional thermal treatment and the machining in the deposition with γ.The volumetric shrinkage that takes place when phase transformation will reduce and the final κ-Al of destruction
2O
3The adhesivity of coating is as U.S. Pat 5700569.Therefore, consider the deposition effect and the abrasion resistance properties (especially when high speed cutting) of coating, α-Al
2O
3Should be best and safest selection mutually, as U.S. Pat 5137774.But, α-Al
2O
3Have the advantages that crystal grain is easily grown up, this is very unfavorable for cutting, causes tipping easily, reduces cutter life.When adopting conventional coatings technology, as α-Al
2O
3When coat-thickness was 7 μ m, crystal grain was very thick, and mean grain size reaches more than the 4 μ m, was difficult to obtain to stablize the α-Al of difficult drop-off
2O
3Thick film coating, and thick aluminum oxide often contains hole and lattice defect.In order to obtain high quality, fine grain α-Al
2O
3Coating adopts the sedimentary method of multilayer substep usually.Adopt the repeatedly sedimentary method of layering as U.S. Pat 6713172 disclosed aluminum oxide, by the next interval of titanium oxide as thin as a wafer, can obtain α-Al of the about 0.5 μ m of surperficial average grain between layer and the layer
2O
3Coating.U.S. Pat 6673393 adopts similar method, obtains the k-Al less than 0.5 μ m
2O
3Coating.U.S. Pat 5071696 is by control nucleation condition and utilize κ-Al
2O
3The meta inversion of phases is α-Al
2O
3Phase obtains fine grain aluminum oxide coating layer, and granular size is between 0.5～2 μ m.
Summary of the invention
The objective of the invention is to overcome technical deficiencies such as alumina grain is thick in the prior art, crystal grain is inhomogeneous, a kind of cutting tool that is applicable to is provided, and formed coating has the preparation method of applying coating on cutter of characteristics such as surface smoothness is higher, uniform crystal particles is finer and closely woven.
The present invention includes following steps:
1) the numerical control blade is put into reaction chamber;
2) reaction chamber is evacuated state;
In step 2) in, the described vacuum tightness that vacuumizes can be below the 10mbar.
3) by heating mantles reaction chamber is heated, adds and depress, feed TiCl
4, N
2And H
2Gaseous mixture, depositing TiN layer on tool surface;
In step 3), the temperature of described heating can be 900～950 ℃, and the pressure of described pressurization can be 50～500mbar; Described TiCl
4, N
2And H
2Gaseous mixture in TiCl by mass percentage
4Be 0.2%～10%, N
2Be 2%～50%, surplus is H
2The thickness of described TiN layer can be 0.5 μ m～1 μ m, and depositing time can be 0.5～1h.
4) deposited the TiN layer after, reaction chamber temperature is stabilized in 850～950 ℃, and under the pressure of 50～500mbar, feed TiCl
4, N
2, CH
3CN and H
2Gaseous mixture, deposition MT-TiCN layer on the TiN laminar surface;
In step 4), described TiCl
4, N2, CH
3CN and H
2Gaseous mixture in TiCl by mass percentage
4Be 0.2%～10%, N
2Be 2%～50%, CH
3CN is 0.2%～10%, and surplus is H
2The thickness of described MT-TiCN layer can be 2～14 μ m, and the sedimentary time can be 1.5～7h.
5) close source of the gas, feed TiCl then
4, AlCl
3, CO, CO
2, CH
4, N
2And H
2Gaseous mixture, be 900～1020 ℃ and be under 50～200mbar in temperature, deposition bonding phase AlTiCNO layer at pressure;
In step 5), described TiCl
4, AlCl
3, CO, CO
2, CH
4, N
2And H
2Gaseous mixture in TiCl by mass percentage
4Be 0.2%～10%, AlCl
3Be 0.2%～8%, CO is 0.3%～9%, CO
2Be 0.1%～5%, CH
4Be 0.2%～7%, N
2Be 0～15%, surplus is H
2The thickness of described bonding phase AlTiCNO layer can be 0.1～1.5 μ m, and the sedimentary time can be 0.2～1h.
6) at TiCl
4, CO, CO
2, CH
4, N
2And H
2Gaseous mixture in, be that 900～1020 ℃ and pressure are under 50～200mbar in temperature, depositing Ti CO layer;
In step 6), described TiCl
4, CO, CO
2, CH
4, N
2And H
2Gaseous mixture in TiCl by mass percentage
4Be 2%～6%, CO is 3%～9%, CO
2Be 1.5%～10%, CH
4Be 0.2%～7%, N
2Be 0～15%, surplus is H
2The thickness of described TiCO layer can be 0.1～0.3 μ m, and the sedimentary time can be 1～30min.
7) at CO
2, AlCl
3, HCl and H
2Gaseous mixture in, be that 900～1020 ℃ and pressure are under 50～200mbar in temperature, the deposition of aluminium oxide nucleating layer;
In step 7), described CO
2, AlCl
3, HCl and H
2Gaseous mixture in CO by mass percentage
2Be 1%～5%, AlCl
3Be 2%～10%, HCl is 1%～15%, and surplus is H
2The thickness of described aluminum oxide nucleating layer can be 0.1～0.8 μ m, and the sedimentary time can be 0.2～1h.
8) feed AlCl
3, CO, CO
2, HCl, H
2S and H
2Gaseous mixture in, be that 900～1020 ℃ and pressure are under 50～200mbar in temperature, deposition of aluminium oxide coatings must apply cated cutter at tool surface.
In step 8), described AlCl
3, CO, CO
2, HCl, H
2S and H
2Gaseous mixture in AlCl by mass percentage
3Be 0.1%～10%, CO is 0～10%, CO
2Be 0～5%, HCl is 0～15%, H
2S is 0.01%～1%, and surplus is H
2The thickness of described aluminum oxide coating layer can be 3～10 μ m, and the sedimentary time can be 4～15h.
Coatings prepared of the present invention comprises one deck α-Al at least
2O
3Layer, α-Al
2O
3Layer is made up of the columnar grain with even fine particle (average grain is less than 1 μ m), and the long-width ratio of columnar grain is 3～13, and is preferred 4～10, and the best is 6～8, and aluminum oxide coating layer thickness is 1～10 μ m, preferred 4～9 μ m.By the scanning electron microscopic observation analysis, granular size is very even, and size distribution is very narrow, and 90% granular size is between 0.75-1.25 μ m.
(Ti, Al) on the CNO, the TiCNO layer of growth-dominated oxygen level on this layer is by regulating Optimization Layer CO at key coat for aluminum oxide coating layer
2And the ratio between the CO is come controlled oxidation atmosphere, makes α-Al
2O
3When forming core, produce a large amount of thin nuclear, thus the crystal grain of refinement aluminum oxide, and in the aluminum oxide developmental process, adopt CO the effective inhibited oxidation aluminum particulate of HCl gas thick, aluminum oxide is grown up uniformly.
One of key that obtains even fine grain aluminum oxide coating layer is control CO and CO in nucleation process
2Ratio, come controlled oxidation atmosphere, this ratio should be 0.1～10, preferably 1～5.Another key is in the aluminum oxide developmental process, adopt CO the effective inhibited oxidation aluminum particulate of HCl gas, this ratio should be 0～15, is preferably 3～6.
The present invention is by regulating Optimization Layer CO
2And the ratio between the CO comes controlled oxidation atmosphere to make α-Al
2O
3Form a large amount of thin nuclear, thus the crystal grain of refinement aluminum oxide, and in the aluminum oxide developmental process, adopt the thick of HCl and the effective inhibited oxidation aluminum particulate of CO gas, aluminum oxide is grown up uniformly.
Description of drawings
Fig. 1 is the section electromicroscopic photograph of coating a aluminum oxide coating layer of the present invention.Aluminum oxide coating layer thickness is about 7 μ m, adopts the way that suppresses to make αYang Hualv form columnar crystal structure.
Fig. 2 is coating a aluminum oxide coating layer of the present invention surface 1k electromicroscopic photograph doubly.As can be seen from Figure 2, the aluminum oxide coating layer surface particles is evenly distributed, and particle is thinner.
Fig. 3 is coating a aluminum oxide coating layer of the present invention surface 5k electromicroscopic photograph doubly.As can be seen from Figure 3, the aluminum oxide size is very even, and it is very concentrated to distribute, and granular size is between 0.75～1.25 μ m.
Fig. 4 is a prior art coating b aluminum oxide coating layer surface 1k electromicroscopic photograph doubly
Fig. 5 is a prior art coating b aluminum oxide coating layer surface 5k electromicroscopic photograph doubly
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
Embodiment 1
Component is 6%Co, and surplus is the carbide cutting blade of WC, and its surface-coated has TiN layer, MT-TiCN layer, and thickness is respectively 0.5～1 μ m, 7 μ m.Also be coated with α-Al that a thickness is about 8 μ m above this layer
2O
3Layer, detailed processing parameter is as shown in table 1.
Table 1
| Step | 1 | 2 | 3 | 4 | 5 | 6 |
| TiN | TiCN | AlTiCNO | TiNCO | Al 2O 3Nucleation | Al 2O 3 | |
| TiCl 4(％) | 1.7 | 1.6 | 4.0 | 2.1 | ||
| N 2(％) | 38 | 35 | 4.0 | 6.0 | ||
| CO 2(％) | 1.8 | 3.0 | 2 | 3 | ||
| CO(％) | 4.0 | 6.0 | 6.0 | |||
| CH 4(％) | 1.0 | 1.0 | ||||
| AlCl 3(％) | 3.0 | 2.8 | 3.2 |
| H 2S(％) | 0.3 | |||||
| HCl(％) | 2 | 2 | ||||
| H 2(％) | Surplus | Surplus | Surplus | Surplus | Surplus | Surplus |
| CH 3CN(％) | 0.9 | |||||
| Pressure (mbar) | 100 | 70 | 150 | 150 | 100 | 70 |
| Temperature (℃) | 930 | 885 | 1000 | 1000 | 1000 | 1000 |
| Time (min) | 60 | 320 | 20 | 20 | 30 | 500 |
Embodiment 2
As a reference, according to the coarse grained aluminium oxide structure of prior art, deposited coatings b, and employing and the same blade base of coating a, same coat-thickness and same blade model.Utilize scanning electron microscope that the aluminum oxide coating layer surface is analyzed.Determine the alumina particle size of coating a and b, as shown in table 2.
Table 2
Embodiment 3
Coating a and coating b are carried out the shock resistance experiment relatively, referring to table 3.
Workpiece: with the cylindrical rod of 4 fault troughs;
Material: 45# steel;
Blade model: WNMG080412;
Cutting parameter: V=200r/min, ap=2mm, F=0.20mm/r.
Table 3
| Sequence number | The trade mark | Time (min) | Impact number of times (inferior) | Remarks |
| 1 | Coating a (the present invention) | 5 | 4000 | Point of a knife is intact |
| 2 | Coating a (the present invention) | 5 | 4000 | Point of a knife is intact |
| 3 | Coating a (the present invention) | 5 | 4000 | Point of a knife is intact |
| 4 | Coating b prior art | 0.2 | 160 | Collapse |
| 5 | Coating b prior art | 1 | 800 | Collapse |
| 6 | Coating b prior art | 1.5 | 1200 | Collapse |
As can be seen from Table 3, the toughness of coating a of the present invention is better than prior art coating b.
Embodiment 4
Coating a and coating b are carried out wear-resisting experiment.
Workpiece: cylindrical rod
Material: HT250 cast iron
Blade model: WNMG080412
Cutting parameter: V=250m/min, ap=1mm, F=0.20mm/r
After adopting cutting 8min, measure the abrasion loss of point of a knife, record numerical value; And then cutting 3min, measure the abrasion loss of point of a knife, and write down the numerical value of corner wear, as shown in table 4.
Table 4
As can be seen from Table 4, the wear resisting property of coating a of the present invention is must prior art coating b good.
Claims (10)
1. the preparation method of an applying coating on cutter is characterized in that may further comprise the steps:
1) the numerical control blade is put into reaction chamber;
2) reaction chamber is evacuated state;
3) by heating mantles reaction chamber is heated, adds and depress, feed TiCl
4, N
2And H
2Gaseous mixture, depositing TiN layer on tool surface;
4) deposited the TiN layer after, reaction chamber temperature is stabilized in 850～950 ℃, and under the pressure of 50～500mbar, feed TiCl
4, N
2, CH
3CN and H
2Gaseous mixture, deposition MT-TiCN layer on the TiN laminar surface;
5) close source of the gas, feed TiCl then
4, AlCl
3, CO, CO
2, CH
4, N
2And H
2Gaseous mixture, be 900～1020 ℃ and be under 50～200mbar in temperature, deposition bonding phase AlTiCNO layer at pressure;
6) at TiCl
4, CO, CO
2, CH
4, N
2And H
2Gaseous mixture in, be that 900～1020 ℃ and pressure are under 50～200mbar in temperature, depositing Ti CO layer;
7) at CO
2, AlCl
3, HCl and H
2Gaseous mixture in, be that 900～1020 ℃ and pressure are under 50～200mbar in temperature, the deposition of aluminium oxide nucleating layer;
8) feed AlCl
3, CO, CO
2, HCl, H
2S and H
2Gaseous mixture in, be that 900～1020 ℃ and pressure are under 50～200mbar in temperature, deposition of aluminium oxide coatings must apply cated cutter at tool surface.
2. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that in step 2) in, the described vacuum tightness that vacuumizes is below the 10mbar.
3. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that in step 3) the temperature of described heating is 900～950 ℃, the pressure of described pressurization is 50～500mbar; Described TiCl
4, N
2And H
2Gaseous mixture in TiCl by mass percentage
4Be 0.2%～10%, N
2Be 2%～50%, surplus is H
2The thickness of described TiN layer can 0.5 μ m～1 μ m, and depositing time is 0.5～1h.
4. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that in step 4) described TiCl
4, N2, CH
3CN and H
2Gaseous mixture in TiCl by mass percentage
4Be 0.2%～10%, N
2Be 2%～50%, CH
3CN is 0.2%～10%, and surplus is H
2The thickness of described MT-TiCN layer is 2～14 μ m, and the sedimentary time is 1.5～7h.
5. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that in step 5) described TiCl
4, AlCl
3, CO, CO
2, CH
4, N
2And H
2Gaseous mixture in TiCl by mass percentage
4Be 0.2%～10%, AlCl
3Be 0.2%～8%, CO is 0.3%～9%, CO
2Be 0.1%～5%, CH
4Be 0.2%～7%, N
2Be 0～15%, surplus is H
2The thickness of described bonding phase AlTiCNO layer is 0.1～1.5 μ m, and the sedimentary time is 0.2～1h.
6. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that in step 6) described TiCl
4, CO, CO
2, CH
4, N
2And H
2Gaseous mixture in TiCl by mass percentage
4Be 2%～6%, CO is 3%～9%, CO
2Be 1.5%～10%, CH
4Be 0.2%～7%, N
2Be 0～15%, surplus is H
2The thickness of described TiCO layer is 0.1～0.3 μ m, and the sedimentary time is 1～30min.
7. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that in step 7) described CO
2, AlCl
3, HCl and H
2Gaseous mixture in CO by mass percentage
2Be 1%～5%, AlCl
3Be 2%～10%, HCl is 1%～15%, and surplus is H
2The thickness of described aluminum oxide nucleating layer is 0.1～0.8 μ m, and the sedimentary time is 0.2～1h.
8. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that in step 8) described AlCl
3, CO, CO
2, HCl, H
2S and H
2Gaseous mixture in AlCl by mass percentage
3Be 0.1%～10%, CO is 0～10%, CO
2Be 0～5%, HCl is 0～15%, H
2S is 0.01%～1%, and surplus is H
2The thickness of described aluminum oxide coating layer is 3～10 μ m, and the sedimentary time is 4～15h.
9. as claimed in claim 1 a kind of on cutter the preparation method of applying coating, it is characterized in that described coating comprises one deck α-Al at least
2O
3Layer, α-Al
2O
3Layer is formed less than the columnar grain of 1 μ m by having average grain, and the long-width ratio of columnar grain is 3～13, and aluminum oxide coating layer thickness is 1～10 μ m.
10. as claimed in claim 9 a kind of on cutter the preparation method of applying coating, the long-width ratio that it is characterized in that described columnar grain is 4～10, the best is 6～8, aluminum oxide coating layer thickness is 4～9 μ m.
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|---|---|---|---|
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|---|---|---|---|
| CN2011100241343A CN102061454B (en) | 2011-01-20 | 2011-01-20 | Method for preparing coating on cutter |
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| CN104053815A (en) * | 2011-12-14 | 2014-09-17 | 山特维克知识产权股份有限公司 | Coated cutting tool and method of manufacturing the same |
| CN104085142A (en) * | 2014-05-28 | 2014-10-08 | 厦门金鹭特种合金有限公司 | Coating layer on blade base body |
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| CN105940141A (en) * | 2014-01-30 | 2016-09-14 | 山特维克知识产权股份有限公司 | Alumina coated cutting tool |
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| US20180274091A1 (en) * | 2017-03-23 | 2018-09-27 | Kennametal Inc. | CONTROL AND CHARACTERIZATION OF TEXTURE IN CVD alpha-Al2O3 COATINGS |
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| CN103173761B (en) * | 2011-12-23 | 2015-08-19 | 株洲钻石切削刀具股份有限公司 | Cutting tool improving coating structure and preparation method thereof |
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| US10570509B2 (en) * | 2014-12-19 | 2020-02-25 | Sandvik Intellectual Property Ab | CVD coated cutting tool |
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| US10865476B2 (en) * | 2017-03-23 | 2020-12-15 | Kennametal Inc. | Control and characterization of texture in CVD α-Al2O3 coatings |
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| CN108411279B (en) * | 2018-03-30 | 2019-07-09 | 华中科技大学 | A kind of preparation method of high-speed steel tool protective coating |
| CN108411279A (en) * | 2018-03-30 | 2018-08-17 | 华中科技大学 | A kind of preparation method of high-speed steel tool protective coating |
| CN110331380A (en) * | 2019-08-06 | 2019-10-15 | 株洲华锐精密工具股份有限公司 | A kind of applying coating and preparation method thereof on blade base |
| CN113512716A (en) * | 2021-03-26 | 2021-10-19 | 四川大学 | Preparation method of titanium carbonitride/aluminum oxide composite coating for repairing substrate |
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