CN103029366A - Product containing NiCrN ternary coating and preparation method thereof - Google Patents
Product containing NiCrN ternary coating and preparation method thereof Download PDFInfo
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- CN103029366A CN103029366A CN2012105287070A CN201210528707A CN103029366A CN 103029366 A CN103029366 A CN 103029366A CN 2012105287070 A CN2012105287070 A CN 2012105287070A CN 201210528707 A CN201210528707 A CN 201210528707A CN 103029366 A CN103029366 A CN 103029366A
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- 238000000576 coating method Methods 0.000 title claims abstract description 100
- 239000011248 coating agent Substances 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims description 18
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 230000007704 transition Effects 0.000 claims abstract description 20
- 238000005121 nitriding Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 17
- 239000000956 alloy Substances 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 14
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 14
- 229910001120 nichrome Inorganic materials 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000012670 alkaline solution Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000005256 carbonitriding Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 abstract description 10
- 239000010959 steel Substances 0.000 abstract description 10
- 239000003960 organic solvent Substances 0.000 abstract description 6
- 238000009736 wetting Methods 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 4
- 230000035939 shock Effects 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 230000004580 weight loss Effects 0.000 abstract description 2
- 238000005299 abrasion Methods 0.000 abstract 2
- 238000000151 deposition Methods 0.000 description 9
- 230000008021 deposition Effects 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000007733 ion plating Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
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- 238000011056 performance test Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
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- 229920003023 plastic Polymers 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000006748 scratching Methods 0.000 description 2
- 230000002393 scratching effect Effects 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- 230000001070 adhesive effect Effects 0.000 description 1
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Abstract
The invention discloses a product containing an NiCrN ternary coating. On the product, a Cr layer is used as a bottom layer, an NiCrN layer is used as a transition layer, and a plurality of NiCrN-CrN composite coatings are deposited on the NiCrN transition layer, so that the thickness of the composite coating reaches 2-5 mu m. By adopting the multilayer gradient design and nitriding technique before filming, the invention greatly enhances the film-base bonding strength of the coating. The critical load of the gradient coating prepared by the invention in a scarification test is up to 75N which is much higher than that of a related coating prepared by any other method or technique; and the hardness of the product containing an NiCrN ternary coating can reach 2780HV. The invention greatly enhances the shock resistance, abrasion resistance, friction resistance and heat stability on the surface of a mold or cutter, and greatly lowers the friction factor and weight loss rate by abrasion. The NiCrN ternary coating greatly enhances the wetting angle of mold steel for organic solvents, which indicates that the coating can greatly improve the demoldability of the mold.
Description
(1) technical field
The present invention relates to a kind of novel PVD ternary coating, be used for improving cutter, die surface hardness, Modificati on and shock-resistant polishing machine, significantly improve cutter, mold use life-span; Improve the demolding performace of die surface, improve working of plastics formed product precision, i.e. a kind of goods and preparation method who contains NiCrN tri compound coating.
(2) background technology
Along with developing rapidly of auto industry, the demand of automobile accessories part increases considerably.Wherein, the quality of workpiece, output and production cost often depend on quality and the Acceptable life of mould.Yet under extremely abominable working condition, early stage surface failure often occurs in mould steel.For preventing mould generation initial failure, prolong the mold use life-span, the most effective most economical mode is carried out surface treatment to mould exactly.The PVD magnetic sputtering coating can effectively improve the surface propertys such as the hardness, antiwear and antifriction of matrix.Wherein, CrTiN tri compound coating has obtained the extensive concern of domestic and international researcher with its excellent mechanical performance.CrTiN tri compound coating has better hardness, film/film-substrate binding strength than present most widely used TiN and CrN.The application of CrTiN coating on the instruments such as drill bit, lathe tool extensively approved, but for mould, the application of this coating but is restricted.This mainly is because the working environment of cutter and mould steel is extremely abominable, and also there is larger defective in CrTiN coating self performance, and for example its toughness is relatively poor, is easy to cracking under shock loading, peels off.For further optimizing properties of coating and improving film substrate bond strength, the present invention introduces the Ni element on the basis of CrTiN coating, is intended to develop a kind of novel NiCrN ternary coating.
(3) summary of the invention
The object of the invention provides a kind of goods and preparation method of the NiCrN of containing ternary coating, further improves the film substrate bond strength of NiCrN composite coating, and the size of controlling each layer tissue crystal grain in the nanoscale scope and evenly; The layer thickness of every one deck is also in the nanoscale scope; The coating structure voidage is low, and dense structure makes coating have best hardness/toughness combination, optimizes shock-resistant polishing machine, antifriction performance and the Modificati on of coating, improves the demolding performace of mould.
The technical solution used in the present invention is:
The invention provides a kind of goods of the NiCrN of containing ternary coating, described goods take the NiCrN layer as transition zone, make the thickness of composite coating reach 2 ~ 5 μ ms at some layers of NiCrN-CrN composite coating of NiCrN transition zone deposition take the Cr layer as bottom.Usually can make the thickness of composite coating reach 2 ~ 5 μ m at NiCrN transition zone deposition NiCrN-CrN composite coating 2 ~ 2.5h.
The present invention also provides a kind of preparation method of the described NiCrN of containing ternary coating goods, described method is: (1) preliminary treatment: with goods substrate ultrasonic cleaning 5 ~ 10min in alkaline solution, ultrasonic cleaning 6 ~ 9min in acetone again, ultrasonic cleaning 4 ~ 8min in absolute ethyl alcohol obtains pretreated goods substrate at last; (2) adopt the non-balance magnetically controlled sputter method, with the Cr layer at Cr target current 3 ~ 5A, substrate bias is-80 ~-120V condition deposit to the pretreated goods substrate as bottom; (3) logical nitrogen, at NiCr alloys target electric current 5 ~ 7A, substrate bias be-40 ~-condition of 80V under, deposit the NiCrN layer as transition zone at bottom; (4) prepare at last the NiCrN-CrN composite coating, logical nitrogen, at Cr target current 5-7A, substrate bias is-50 ~-80V, NiCr alloys target electric current 4 ~ 6A, substrate bias is-50 ~-the 80V condition under, the NiCrN-CrN composite coating deposited to make NiCrN-CrN composite coating thickness on the transition zone be 2 ~ 5 μ m, namely obtain to contain the goods of NiCrN ternary coating.
Further, the described method of step (1) is: with goods substrate ultrasonic cleaning 8min in alkaline solution, and ultrasonic cleaning 9min in acetone again, ultrasonic cleaning 8min in absolute ethyl alcohol obtains pretreated goods substrate at last; Described alkaline solution is the 10g/L alkaline aqueous solution, and described alkaline aqueous solution neutral and alkali material is NaOH.
Further, the described preprocessing process of step (1) also comprises the goods substrate in absolute ethyl alcohol behind ultrasonic cleaning 4 ~ 8min, carries out nitriding processing or carbo-nitriding again and processes.It is to well known to a person skilled in the art method that nitriding processing or carbo-nitriding are processed, and nitriding is processed and referred to mould steel 570 ℃ of lower nitridings in nitriding furnace were processed 8 hours usually; The carbo-nitriding processing is to point to the process that the top layer of steel is infiltrated carbon and nitrogen simultaneously.
Further, step (2) adopts the non-balance magnetically controlled sputter method that Cr is deposited on the pretreated goods substrate as bottom, and sedimentary condition is: Cr target current 3 ~ 5A, substrate bias is-100V.
Further, step (3) adopts magnetron sputtering method that NiCrN is deposited on the Cr bottom as transition zone, and sedimentary condition is: logical nitrogen, and NiCr alloys target electric current 6A, substrate bias is-65V.
Further, step (4) adopts the non-balance magnetically controlled sputter method that the NiCrN-CrN composite coating is deposited to and makes the goods that contain (NiCrN-CrN) compound ternary coating on the NiCrN transition zone, sedimentary condition is: at Cr target current 6A, substrate bias is-65V, NiCr alloys target electric current 5A, substrate bias is-65V.Wherein (NiCrN-CrN) composite coating deposition is with the deposition basis of transition zone.
The present invention designs preparation multi-layer nano gradient coating, to improve the film substrate bond strength of coating, at the basis of CrTiN composite coating Ni element substitution Ti, the Ni element can improve coating toughness and heat endurance to a great extent, and can reduce the wetness degree of mould and liquid plastic; Before plated film, increase nitridation process or carry out the carbo-nitriding processing.Workpiece running status in stove is that diaxon rotates, and namely around the main shaft revolution, also finishes rotation simultaneously.
Cr target of the present invention, the NiCr alloys target is high pure metal, recommends the ladder that coating company available from Britain.
Compared with prior art, beneficial effect of the present invention is mainly reflected in:
(1) the present invention adopts multi-gradient design and the front nitridation process of plated film greatly to improve the film substrate bond strength of coating, the critical load of gradient coating in scratch test of the present invention preparation up to the general film substrate bond strength of 75N(about 45N), far above the relevant coating of other Method and process preparation;
(2) owing to the existence in the rich Ni of disperse district, dispersion-strengtherning and stress reinforced effect strengthen by regulating the electric current of NiCr alloys target in the coating, make the hardness that contains NiCrN ternary coating goods can reach 2780HV;
(3) the Ni element has improved the toughness of coating to a great extent, can obtain optimum hardness/toughness combination by control preparation technology, and the existence of Ni makes the coated grains refinement, and porosity reduces, and compactness improves;
(4) the NiCrN ternary coating has significantly improved impact-resistant abrasion-proof antifriction performance and the heat endurance of mould and tool surface, and coefficient of friction and wear weight loss rate all significantly reduce;
(5) the NiCrN ternary coating has improved the angle of wetting of mould steel to organic solvent greatly, shows that this coating can significantly improve the demolding performace of mould.
(4) description of drawings
The coating structure schematic diagram of Fig. 1 the present invention preparation.
Fig. 2 target distributes and places schematic diagram with specimen holder.
Fig. 3 Teer-UDP850/4 type magnetic control sputtering device photo.
Fig. 4 contains the scanning electron microscope (SEM) photograph of NiCrN ternary coating product surface.
Fig. 5 contains the angle of wetting of NiCrN ternary coating goods organic solvent.
Fig. 6 is without the angle of wetting of coated article surface organic solvent.
(5) specific embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
The Teer-UDP850/4 type closed field unbalanced magnetron sputtering ion plating equipment (Teer-UDP850/4 closed-filed unbalanced magnetron sputtering ion plating coater) of selecting your coating company of Britain's ladder to make prepares the goods of the CrNiN of containing ternary coating of the present invention, this equipment is comprised of vacuum system, power-supply system, control system, cooling system four parts, and photo as shown in Figure 3.
Vacuum system is two-stage vacuum, and prime adopts mechanical pump slightly to take out, and rear class adopts the diffusion pump essence to take out.As shown in Figure 2, four targets (2 Cr targets, 2 NiCr alloys target are all available from Britain ladder that coating company) are installed on the vacuum wall.
Embodiment 1
(1) substrate preliminary treatment: take with H13 mould steel as the goods substrate, with goods substrate ultrasonic cleaning 8min in 10 g/L sodium hydrate aqueous solutions, ultrasonic cleaning 9min in acetone again, ultrasonic cleaning 8min in absolute ethyl alcohol obtains pretreated goods substrate at last.
(2) adopt Teer-UDP850/4 type closed field unbalanced magnetron sputtering ion plating equipment to prepare the key step of NiCrN ternary coating (the coating structure schematic diagram is as shown in Figure 1) as follows:
1) start preheating, logical cooling water is opened mechanical pump and is evacuated to 4.0 * 10
-4Pa, and vacuum chamber is heated to 100 ℃;
2) pass into argon gas, regulate gas cylinder valve and flowmeter, adjust the vacuum chamber internal gas pressure and make the target build-up of luminance;
3) Ion Cleaning: make the matrix rotation, regulate substrate bias to 400V, clean matrix surface 20min with Ar+, remove surface impurity, for formal plated film is prepared;
4) plated metal Cr bottoming: open the Cr target, target current is 4A, adjusts substrate bias to be-100V, and deposition one deck Cr is as bottom, to improve the bond strength of coating and matrix;
5) deposition NiCrN transition zone: NiCr alloys target electric current is increased to 6 A, and substrate bias-65V opens the nitrogen valve, and deposition layer of Ni CrN is as transition zone, with the bond strength of further enhancing coating and matrix;
6) deposition (NiCrN-CrN) composite coating: four targets (2 Cr targets, 2 NiCr alloys target) are all opened by arrangement shown in Figure 2, logical nitrogen, and the Cr target current is 6A, substrate bias-65V, NiCr alloys target electric current is 5A, substrate bias-65V.
7) plated film is complete: cool off after 30 minutes, and applying argon gas, blow-on, sampling, NiCrN-CrN composite coating thickness is 3 μ m in the goods, namely obtain to contain the goods of NiCrN ternary coating, and the goods that will contain the NiCrN ternary coating carries out performance test as sample.Concrete technological parameter is shown in Table 1.
The preparation technology parameter of table 1 CrNiN ternary coating
Adopt HMV-1T type microhardness testers, measure the microhardness value under the 10g load, hold time is 10s.In order to reduce each sample measurement microhardness value of error five times, get five times arithmetic mean of instantaneous value as the hardness number of this sample.The microhardness value that contains the NiCrN ternary coating can reach 2580HV.
Adopting CQY-18 type ball trace instrument to measure and calculating the thickness that contains NiCrN ternary coating goods floating coat is 3 μ m; Adopt the film substrate bond strength of WS-2004 type coating adhesion scratching instrument characterizing coating, the critical load in the scratch test is 60N.
The NiCrN ternary coating of the present invention's preparation has rational component gradient structure, the structural design of coating is as shown in Figure 1: because Cr and steel matrix have the good adhesive force of generally acknowledging, so at first use the Cr bottoming, then use the NiCrN transition on it, deposition has the NiCrN-CrN composite bed film of nano-multilayered structures at last.Physics, chemical property and the institutional framework that the membranous layer ingredient of this continuously smooth transition can make rete be continuous transition gradually, alleviates stress state at the interface, thereby can improve to a great extent the combination property of film.
Embodiment 2
The 570 ℃ of lower nitridings in nitriding furnace of pretreated H13 mould steel were processed 8 hours, then adopted Teer-UDP850/4 type closed field unbalanced magnetron sputtering ion plating equipment to prepare the NiCrN ternary coating.Other operations and method are with embodiment 1, and NiCrN-CrN composite coating thickness is 3 μ m in the goods, namely obtain to contain the goods of NiCrN ternary coating, and the goods that will contain the NiCrN ternary coating carry out performance test as sample.
The VEGA-3-S type SEM that adopts Czech TESCAN company to produce is observed the specimen surface pattern, the results are shown in shown in Figure 4.Fig. 4 has shown NiCrN ternary coating nano surface crystalline form looks.
Adopt HMV-1T type microhardness testers, measure the microhardness value under the 10g load, hold time is 10s.In order to reduce each sample measurement microhardness value of error five times, get five times arithmetic mean of instantaneous value as the hardness number of this sample.The microhardness value of coating can reach 2780HV.
Adopting CQY-18 type ball trace instrument to measure the thickness that calculates coating is 3 μ m; Adopt the film substrate bond strength of WS-2004 type coating adhesion scratching instrument characterizing coating, the critical load in the scratch test is 75N.
Adopting the luxuriant and rich with fragrance QCA35 type of German moral contact angle measurement to measure mould steel surface NiCrN ternary coating organic solvent angle of wetting is 101.9 degree (Fig. 5), and without angle of wetting 78.3 degree (Fig. 6) of coating mold surface organic solvent, show that this coating can significantly improve the demolding performace of mould.
Claims (7)
1. goods that contain the NiCrN ternary coating is characterized in that described goods take the Cr layer as bottom, and take the NiCrN layer as transition zone, deposit thickness is the NiCrN-CrN composite coating of 2 ~ 5 μ m on the NiCrN layer.
2. described preparation method who contains NiCrN ternary coating goods of claim 1, it is characterized in that described method is: 1) preliminary treatment: with goods substrate ultrasonic cleaning 5 ~ 10min in alkaline solution, ultrasonic cleaning 6 ~ 9min in acetone again, ultrasonic cleaning 4 ~ 8min in absolute ethyl alcohol obtains pretreated goods substrate at last; (2) adopt the non-balance magnetically controlled sputter method, with the Cr layer at Cr target current 3 ~ 5A, substrate bias is-80 ~-120V condition deposit to the pretreated goods substrate as bottom; (3) logical nitrogen, at NiCr alloys target electric current 5 ~ 7A, substrate bias be-40 ~-condition of 80V under, deposit the NiCrN layer as transition zone at bottom; (4) logical nitrogen, at Cr target current 5 ~ 7A, substrate bias is-50 ~-80V, NiCr alloys target electric current 4 ~ 6A, substrate bias is-50 ~-80V, under the condition, the NiCrN-CrN composite coating deposited to make NiCrN-CrN composite coating thickness on the transition zone be 2 ~ 5 μ m, namely obtain to contain the goods of NiCrN ternary coating.
3. the preparation method who contains as claimed in claim 2 NiCrN ternary coating goods, it is characterized in that the described method of step (1) is: with goods substrate ultrasonic cleaning 8min in alkaline solution, ultrasonic cleaning 9min in acetone again, ultrasonic cleaning 8min in absolute ethyl alcohol obtains pretreated goods substrate at last; Described alkaline solution is the 10g/L alkaline aqueous solution, and described alkaline aqueous solution neutral and alkali material is NaOH.
4. as containing the preparation method of NiCrN ternary coating goods as described in claim 2 or 3, it is characterized in that the described preprocessing process of step (1) also comprises behind ultrasonic cleaning 4 ~ 8min, carries out substrate again nitriding processing or carbo-nitriding and processes in absolute ethyl alcohol.
5. the preparation method who contains as claimed in claim 2 NiCrN ternary coating goods, it is characterized in that step (2) adopts the non-balance magnetically controlled sputter method that Cr is deposited on the pretreated goods substrate as bottom, sedimentary condition is: Cr target current 3 ~ 5A, substrate bias is-100V.
6. the preparation method who contains as claimed in claim 2 NiCrN ternary coating goods is characterized in that step (3) is deposited on the bottom NiCrN as transition zone, and sedimentary condition is: logical nitrogen, and NiCr alloys target electric current 6A, substrate bias is-65V.
7. the preparation method who contains as claimed in claim 2 NiCrN ternary coating goods, it is characterized in that step (4) deposits to the NiCrN-CrN composite coating makes the goods that contain NiCrN tri compound coating on the NiCrN transition zone, sedimentary condition is: at Cr target current 6A, substrate bias is-65V, NiCr alloys target electric current 5A, substrate bias is-65V.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104328385A (en) * | 2014-10-24 | 2015-02-04 | 北京机械工业自动化研究所 | Preparation method of compressor blade coating and surface modifier |
| CN104862644A (en) * | 2015-05-22 | 2015-08-26 | 浙江工业大学 | Cr-CrN-CrMoAlN gradient nano multi-layered thin film with high-temperature wear resistance and preparation method thereof |
| CN107151786A (en) * | 2017-06-06 | 2017-09-12 | 南京林业大学 | A kind of soft or hard composite coating wood cutter and preparation method thereof |
| CN108193173A (en) * | 2017-12-29 | 2018-06-22 | 马鞍山市安工大工业技术研究院有限公司 | Multilayer composite coating of low-adhesion tire mold and preparation method thereof |
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| CN104862644A (en) * | 2015-05-22 | 2015-08-26 | 浙江工业大学 | Cr-CrN-CrMoAlN gradient nano multi-layered thin film with high-temperature wear resistance and preparation method thereof |
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