CN102634760A - Coating and production method thereof - Google Patents
Coating and production method thereof Download PDFInfo
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- CN102634760A CN102634760A CN2011100442785A CN201110044278A CN102634760A CN 102634760 A CN102634760 A CN 102634760A CN 2011100442785 A CN2011100442785 A CN 2011100442785A CN 201110044278 A CN201110044278 A CN 201110044278A CN 102634760 A CN102634760 A CN 102634760A
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Abstract
The invention provides a coating, which comprises a hard base, a transition layer, a composite hard layer and an antioxidant layer, wherein the transition layer, the composite hard layer and the antioxidant layer are formed sequentially on the hard base. The transition layer is a chromium layer. The composite hard layer is composed of a chromium nitride layer and a hafnium nitride layer. The antioxidant layer is an aluminum oxide layer. In addition, the invention provides a production method of the coating, which includes the steps of providing the hard base, and sequentially forming the transition layer, the composite hard layer and the antioxidant layer on the hard base by magnetron sputtering. The coating produced by the method is high in hardness and fine in oxidation resistance.
Description
Technical field
The present invention relates to a kind of lining part and method of manufacture thereof.
Background technology
Technique for vacuum coating has a wide range of applications at industrial circle, wherein, and TiN film plated work-ing life of significantly improving cutter and mould at cutter or mold surface energy.Yet, along with metal cutting processing develops towards high cutting speed, high speed of feed, high reliability, long lifetime, high precision and the good controlled aspect of cutting, to surface-coated demands for higher performance.Traditional single tin lining part can not meet the demands at aspects such as hardness, toughness.
The ZrN film gets more and more people's extensive concerning owing to its hardness and toughness all are superior to the TiN film.But single ZrN film has not almost had the space of raising at aspects such as hardness, oxidation-resistances, is difficult to satisfy the demand of modern industry.Know that again CrN is a kind of hard thin film material, can be used as superhard tool material and surface protecting material.But because the hardness not very high (about 18GPa) of CrN itself; Its application on cutter or mould is restricted; In addition; The oxidation-resistance poor effect of above-mentioned ZrN or CrN ganoine thin film, plating can not play good antioxygenation in cutter or die surface, causes the inefficacy of film easily.
Summary of the invention
Given this, be necessary to provide a kind of lining part that had not only had high firmness but also had preferable antioxidant property.
A kind of method of manufacture of above-mentioned lining part also is provided in addition.
A kind of lining part; This lining part comprises hard substrate; Be formed at transition layer, composite ganoine layer and anti oxidation layer on this hard substrate successively; Said transition layer is the chromium layer, and said composite ganoine layer comprises chromium nitride layer and the nitrogenize hafnium layer that is formed at successively on the transition layer, and said anti oxidation layer is an alumina layer.
A kind of method of manufacture of the part that is covered may further comprise the steps:
One hard substrate is provided;
Surface magnetic control sputtering chromium layer in this hard substrate;
Magnetron sputtering chromium nitride layer on this chromium layer;
Magnetron sputtering nitrogenize hafnium layer on this chromium nitride layer;
Magnetron sputtering alumina layer on this nitrogenize hafnium layer.
Said chromium layer plays adhewsive action to the chromium nitride layer in the composite ganoine layer, and it can combine hard substrate and composite ganoine layer well more firmly.But the chromium nitride layer that forms successively in the meanwhile said composite ganoine layer combines the composite ganoine layer more firm with the nitrogenize hafnium layer; Mainly be because chromium nitride layer has stronger adhesive ability performance; It has the thermal expansivity more close with hard substrate as outermost hafnium nitride tool simultaneously; Therefore internal stress is little at the interface, thus make its with the bonding force of chromium nitride layer more by force, toughness is higher, and the thermostability of hafnium nitride and chemicalstability all are better than other hard layer material; So sputter chromium nitride and nitrogenize hafnium layer can significantly improve the hardness and the anti-deciduous of rete of the part that is covered successively in sputter on the lining part.At last, at this composite ganoine layer magnetron sputtering alumina layer, it brings better antioxidant property can for above-mentioned composite ganoine layer, thereby has prolonged the work-ing life of product.
Description of drawings
Fig. 1 is the sectional view of the lining part of preferred embodiment of the present invention;
Fig. 2 is the schematic top plan view of the used vacuum plating unit of lining part in the shop drawings 1.
The main element nomenclature
Lining part 10
Composite ganoine layer 15
Nitrogenize hafnium layer 153
Source of the gas passage 24
Embodiment
See also Fig. 1, the lining part 10 of the present invention's one preferred embodiment comprises a hard substrate 11, and is formed at transition layer 13, composite ganoine layer 15 and the anti oxidation layer 17 on this hard substrate 11 successively.
This transition layer 13 is the chromium layer.
This composite ganoine layer 15 comprises the chromium nitride layer 151 and nitrogenize hafnium layer 153 that is formed at successively on the hard substrate 11.This chromium nitride layer 151 can form through the mode of magnetron sputtering with nitrogenize hafnium layer 153.
This anti oxidation layer 17 is an alumina layer.
In the present embodiment, the thickness of this composite ganoine layer 15 is 3～7 μ m.
The material of this hard substrate 11 can be hard metals such as rapid steel, wimet and stainless steel.
Lining part 10 in the present embodiment can be all kinds of cutting tools, precision measuringtoll or mould.
The method of making said lining part 10 mainly comprises the steps:
This hard substrate 11 is carried out pre-treatment.
Said hard substrate 11 is put into the ultrasonic cleaner that is loaded with ethanol or acetone soln shake cleaning, to remove the impurity and the greasy dirt on hard substrate 11 surfaces.Dry for standby after cleaning finishes.
Argon plasma is carried out on the surface of the hard substrate after above-mentioned processing 11 clean, further remove the greasy dirt on hard substrate 11 surfaces, to improve hard substrate 11 surfaces and follow-up coating's adhesion.
One coating equipment 100 is provided; Coating equipment 100 comprises that a coating chamber 20 and is used for the vacuum pump 30 that this coating chamber 20 is vacuumized; Be provided with pivoted frame (not shown) in this coating chamber 20; Hard substrate 11 is fixed on the pivoted frame, and pivoted frame drives hard substrate 11 along circular trace 21 revolution, and hard substrate 11 also rotation along track 21 revolution the time.On these coating chamber 20 sidewalls, chromium target 22, aluminium target 23 are installed respectively, and chromium target 22, aluminium target 23 both are symmetrical about the center of track 21.Two ends at chromium target 22, aluminium target 23 are provided with source of the gas passage 24, and gas blows out the surface of bombardment chromium target 22, aluminium target 23 via this source of the gas passage 24, so that chromium target 22, aluminium target 23 surface sputterings go out particle.When hard substrate 11 passes through chromium target 22, aluminium target 23 respectively, with the particle that plates chromium target 22, aluminium target 23 surface sputterings.
Concrete operations and processing parameter that this plasma cleans can be: to this coating chamber 20 vacuumize handle to vacuum tightness be 8.0 * 10
-3Pa; In coating chamber 20, feeding purity with the flow of 300～500sccm (standard state ml/min) is 99.999% argon gas (working gas); On hard substrate 11, apply-300～-bias voltage of 800V; In said coating chamber 20, form high-frequency voltage, make said argon gas ionization and produce argon plasma physical bombardment is carried out on the surface of hard substrate 11, and reach purpose hard substrate 11 surface cleaning.The time that said argon plasma cleans is 3～10min.
After hard substrate 11 being carried out the plasma cleaning, on this hard substrate 11, form said transition layer 13.The concrete operations and the processing parameter that form this transition layer 13 are following: be working gas with the argon gas; The adjusting argon flow amount is 100～300sccm, on hard substrate 11, apply-50～-bias voltage of 200V, the dutycycle that bias voltage is set is 30%～80%; And 20 to 100～150 ℃ of coating chambers of heating; With chromium target 22 is target, and it is 8～13kw that its power is set, deposition transition layer 13.This transition layer is a chromium layer.The time that deposits this transition layer 13 is 10～30min.
On this transition layer 13, form composite ganoine layer 15.At first form the chromium nitride layer 151 in the said composite ganoine layer 15.The concrete operations and the processing parameter that form this chromium nitride layer 151 are following: be working gas with the argon gas; The adjusting argon flow amount is 100～300sccm; Feeding flow is the reactant gases nitrogen of 10～70sccm; On hard substrate 11, apply-50～-bias voltage of 200V, the dutycycle that bias voltage is set is 30%～80%, and 20 to 100～150 ℃ of heating coating chambers; Open chromium target 22, it is 1～3kw that its power is set, sedimenting chromium chloride layer 151.The time that deposits this chromium nitride layer 151 is 10～30min.
On this chromium nitride layer 151, form nitrogenize hafnium layer 153, concrete operations and processing parameter are following: be working gas with the argon gas, in said coating chamber 20, feeding flow is the reactant gases nitrogen of 10～70sccm; With hafnium target 23 is target, and the power that hafnium target 23 is set is 1～4KW, the bias voltage that puts on hard substrate 11 is-100～-300V; The dutycycle that bias voltage is set is 30%～80%; Nitrogen flow is 10～70sccm, and sputter temperature is 100～200 ℃, deposits said nitrogenize hafnium layer 153.The time that deposits this nitrogenize hafnium layer 153 is 60～90min.
On this composite ganoine layer 15, form anti oxidation layer 17; Its concrete operations and processing parameter are following: with the argon gas is working gas, and it is 100～200sccm that argon flow amount is set, and is reactant gases with oxygen; It is 150～200sccm that oxygen flow is set; To hard substrate 11 apply-50～-bias voltage of 100V, the dutycycle that bias voltage is set is 30%～50%, and heating coating chamber to 100～150 ℃; Open aluminium target 22, it is 8～13kw that its power is set, aluminum oxide layer 17.The time of aluminum oxide layer 17 is 30～60min.The thickness of controlled oxidation aluminium lamination 17 is 0.5～1.0 μ m.
Describe below in conjunction with the preparation method and the lining part 10 of specific embodiment lining part 10:
Embodiment 1
Plasma cleans: argon flow amount is 280sccm, and the bias voltage of hard substrate 11 is-300V that the time that plasma cleans is 9 minutes;
Sputter transition layer 13: feed argon gas 100sccm, the bias voltage-50V that on hard substrate 11, applies opens chromium target 22, and it is 8kw that its power is set, and depositing time is 10min.
Sputter chromium nitride layer 151: feed argon gas 100sccm, nitrogen flow is 10sccm, opens chromium target 22, and it is 1kw that its power is set, and the bias voltage that hard substrate 11 is applied is-100V to deposit 20 minutes;
Sputter nitrogenize hafnium layer 153: feed argon gas 100sccm, nitrogen flow is 10sccm, opens hafnium target 23 on hard substrate 11, to apply-bias voltage of 100V, deposits 60 minutes.
Sputter anti oxidation layer 17: with the argon gas is working gas, and its flow is 150sccm, is reactant gases with oxygen, and the flow that oxygen is set is 50sccm, on hard substrate 11, applies-bias voltage of 50V, and depositing time is 30min.
Embodiment 2
Plasma cleans: argon flow amount is 280sccm, and the bias voltage of hard substrate 11 is-300V that the time that plasma cleans is 9 minutes;
Sputter transition layer 13: feed argon gas 100sccm, the bias voltage-100V that on hard substrate 11, applies opens chromium target 22, and it is 10kw that its power is set, and depositing time is 20min.
Sputter chromium nitride layer 151: feed argon gas 100sccm, nitrogen flow is 40sccm, opens chromium target 22, and it is 2kw that its power is set, and the bias voltage that hard substrate 11 is set is-150V to deposit 25 minutes;
Sputter nitrogenize hafnium layer 153:, feed argon gas 100sccm, nitrogen 40sccm is set, open hafnium target 23 on hard substrate 11, to apply-bias voltage of 200V, deposit 70 minutes.
Anti oxidation layer 17: with the argon gas is working gas, and its flow is 150sccm, is reactant gases with oxygen, and the flow that oxygen is set is 100sccm, on hard substrate 11, applies-bias voltage of 100V, and depositing time is 50min.
Embodiment 3
Plasma cleans: argon flow amount is 280sccm, and the bias voltage of hard substrate 11 is-300V that the time that plasma cleans is 9 minutes;
Sputter transition layer 13: feed argon gas 100sccm, the bias voltage-100V that on hard substrate 11, applies opens chromium target 22, and it is 13kw that its power is set, and depositing time is 30min.
Sputter chromium nitride layer 151: feed argon gas 100sccm, nitrogen flow is 70sccm, opens chromium target 22, and it is 3kw that its power is set, and the bias voltage that hard substrate 11 is set is-300V to deposit 30 minutes;
Sputter nitrogenize hafnium layer 153: feed argon gas 100sccm, nitrogen flow is 70sccm, opens hafnium target 23 on hard substrate 11, to apply-bias voltage of 300V, deposits 90 minutes.
Anti oxidation layer 17: with the argon gas is working gas, and its flow is 150sccm, is reactant gases with oxygen, and the flow that oxygen is set is respectively 75sccm, on hard substrate 11, applies-bias voltage of 150V, and depositing time is 60min.
The performance test of lining part 10
(1) hardness test, concrete testing method is following:
Adopting MVK-H11 type Vickers hardness tester, is under the effect of 0.025kg power in load, the Vickers' hardness of test lining part 10.
The result shows, is respectively 621HV, 630HV and 634HV by the Vickers' hardness of the lining part 10 of the embodiment of the invention 1 to 3 manufacturing.It is thus clear that this lining part 10 has higher hardness.
(2) high-temperature oxidation resistant test, concrete testing method is following:
The testing tool that adopts is the tubular type heat treatment furnace, and test condition is: temperature rise rate is 10 ℃/min, and thermal treatment temp is 800 ℃, and soaking time is 10h.
Test result shows, by the embodiment of the invention 1 to 3 prepared lining part 10 behind 800 ℃ of thermal treatment 10h, all do not see oxidation, come off etc. bad.
Claims (9)
- One kind the lining part; It is characterized in that: this lining part comprises hard substrate; Be formed at transition layer, composite ganoine layer and anti oxidation layer on this hard substrate successively; Said transition layer is the chromium layer, and said composite ganoine layer comprises chromium nitride layer and the nitrogenize hafnium layer that is formed at successively on the transition layer, and said anti oxidation layer is an alumina layer.
- 2. lining part as claimed in claim 1 is characterized in that: the thickness of this composite ganoine layer is 3～7 μ m.
- 3. lining part as claimed in claim 1 is characterized in that: the material of this hard substrate is rapid steel and stainless steel.
- 4. the preparation method of the part that is covered may further comprise the steps:One hard substrate is provided;Surface magnetic control sputtering chromium layer in this hard substrate;Magnetron sputtering chromium nitride layer on this chromium layer;Magnetron sputtering nitrogenize hafnium layer on this chromium nitride layer;Magnetron sputtering alumina layer on this nitrogenize hafnium layer.
- 5. the preparation method of lining part as claimed in claim 4 is characterized in that: the magnetron sputtering chromium nitride layer is a working gas with the argon gas; The adjusting argon flow amount is 100～300sccm; Feeding flow is the nitrogen of 10～70sccm, to hard substrate apply bias voltage-50～-200V, the dutycycle that bias voltage is set is 30%～80%; Open chromium target, it is 1～3kw that its power is set.
- 6. the preparation method of lining part as claimed in claim 5 is characterized in that: the time of the said chromium nitride layer of magnetron sputtering is 20～30min.
- 7. the preparation method of lining part as claimed in claim 4; It is characterized in that: the processing parameter that forms this nitrogenize hafnium layer is: with the hafnium target is target; The power that the hafnium target is set is 1～4KW; Hard substrate is applied bias voltage is-100～-300V, the dutycycle that bias voltage is set is 30%～80%, nitrogen flow is 10～70sccm.
- 8. the preparation method of lining part as claimed in claim 7 is characterized in that: the time of the said nitrogenize hafnium layer of magnetron sputtering is 60～90min.
- 9. the preparation method of lining part as claimed in claim 4; It is characterized in that: the technology of magnetron sputtering alumina layer: it is 100～200sccm that argon flow amount is set, and it is 150～200sccm that oxygen flow is set, to hard substrate apply-50～-bias voltage of 100V; The dutycycle that bias voltage is set is 30%～50%; Selection aluminium is target, and it is 8～13kw that its power is set, and depositing time is 30～60min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100442785A CN102634760A (en) | 2011-02-15 | 2011-02-15 | Coating and production method thereof |
| TW100106744A TW201233825A (en) | 2011-02-15 | 2011-03-01 | Coating and method for manufacturing the coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100442785A CN102634760A (en) | 2011-02-15 | 2011-02-15 | Coating and production method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102634760A true CN102634760A (en) | 2012-08-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100442785A Pending CN102634760A (en) | 2011-02-15 | 2011-02-15 | Coating and production method thereof |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN102634760A (en) |
| TW (1) | TW201233825A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815657A (en) * | 2017-11-07 | 2018-03-20 | 福建工程学院 | A kind of alumina ceramic coating of Color tunable and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002014568A2 (en) * | 2000-08-11 | 2002-02-21 | Kennametal Inc. | Chromium-containing cemented carbide body having a surface zone of binder enrichment |
-
2011
- 2011-02-15 CN CN2011100442785A patent/CN102634760A/en active Pending
- 2011-03-01 TW TW100106744A patent/TW201233825A/en unknown
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002014568A2 (en) * | 2000-08-11 | 2002-02-21 | Kennametal Inc. | Chromium-containing cemented carbide body having a surface zone of binder enrichment |
Non-Patent Citations (3)
| Title |
|---|
| 余东海等: "刀具涂层材料研究进展", 《工具技术》 * |
| 李瑞玲: "磁控溅射CrN/W2N多层薄膜和Ti/a-C复合薄膜的结构调控及摩擦学性能", 《中国优秀硕士学位论文全文数据库》 * |
| 闻立时等: "离子镀硬质膜技术的最新进展和展望", 《真空》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815657A (en) * | 2017-11-07 | 2018-03-20 | 福建工程学院 | A kind of alumina ceramic coating of Color tunable and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| TW201233825A (en) | 2012-08-16 |
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Application publication date: 20120815 |