CN114059029B - Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing and preparation method thereof - Google Patents
Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing and a preparation method thereof, and the preparation method sequentially comprises the following steps: (1) Regulating the vacuum degree, introducing argon, and depositing a Cr transition layer on the surface of the pretreated substrate to obtain the Cr transition layer; (2) Introducing nitrogen, and depositing a CrN transition layer on the Cr transition layer to obtain the CrN transition layer; (3) Alternately depositing NbN and NbXN nano layers in Ar/N2 atmosphere, naturally cooling to room temperature after deposition, and turning off a power supply and a gas source to obtain the Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing. The invention also comprises the rare earth superlattice coating prepared by the method. The invention improves the hardness, binding force, high thermal stability, corrosion resistance and wear resistance of the coating, and prolongs the service life while guaranteeing the cutting quality.
Description
Technical Field
The invention belongs to the technical field of superlattice coating preparation, and particularly relates to a Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing and a preparation method thereof.
Background
With the vigorous development of the processing industry, the demand for high temperature alloys with excellent comprehensive properties in industrial production has increased dramatically, but the difficulty in processing is a great difficulty faced by it. In the face of this dilemma, cemented carbide tool coatings have also evolved towards high hardness, good chemical stability, high temperature oxidation resistance, and excellent thermal stability. The coating composition and structure are updated, the element composition is diversified, the layer number of the coating is increased, and the microstructure tends to be nano from a columnar crystal structure. The common binary and ternary coatings comprise three kinds of nitride, carbide and oxide, and currently mainly comprise TiAlN-based nitride, but the defects of low hardness, high wear rate, poor oxidation resistance and the like are difficult to meet the requirements of the processing industry when difficult-to-process materials such as high-temperature alloy and the like are processed.
The NbN coating is seen into the field of view of people due to the ultrahigh superconducting critical transition temperature, and the excellent mechanical property of NbN is also the key point of research along with the research, and the hardness of the NbN film deposited on a cutter by ion beam assisted deposition and magnetron sputtering is more than 30Gpa, and the friction coefficient is lower than 0.5. In addition, the nano multi-layer film related to NbN can show more excellent hardness, lower friction coefficient and good chemical stability, so that the NbN coating is successfully and widely applied to the field of hard cutting coatings.
In recent years, tiN/NbN nano multi-layer films with good mechanical properties and chemical stability are widely focused in industrial production. The TiN/NbN nano multilayer film mainly comprises a face-centered cubic NbN phase and a face-centered cubic TiN phase, the hardness can reach 40GPa and the elastic modulus can reach 465GPa by utilizing an excellent periodic layered structure, but the overall abrasion of the coating is poor, the friction coefficient is above 0.5, and the coating can be worn out in long-term cutting. Although researchers invent NbBN composite coatings and the wear rate is reduced, the microhardness is only 31GPa; the elastic modulus decreases to 366GPa, which is a serious impairment of the overall properties of the tool coating.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing and the preparation method thereof, which improve the hardness, binding force, high thermal stability, corrosion resistance and wear resistance of the coating, ensure the cutting quality and prolong the service life.
In order to achieve the above purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing comprises the following steps in sequence:
(1) Regulating the vacuum degree to 0.25-0.4Pa, introducing argon to 40-70sccm, and keeping the sputtering power of the Cr target at 300-400W, wherein the negative bias voltage of the substrate is kept at 40-200V, the deposition time is 10-20min, and depositing a Cr transition layer on the surface of the pretreated substrate to obtain the Cr transition layer;
(2) Introducing nitrogen, controlling the total pressure of the vacuum chamber to be 0.3-0.5Pa, ar and N 2 The partial pressure ratio is 5:1-2, the sputtering power of the Cr target is 300-500W, the negative bias voltage of the matrix is kept at 40-200V, the deposition time is 10-20min, and a CrN transition layer is deposited on the Cr transition layer obtained in the step (1) to obtain the CrN transition layer;
(3) In Ar/N 2 Alternately depositing NbN and NbXN nano layers in the atmosphere, naturally cooling to room temperature after deposition, closing a power supply and a gas source, and obtaining the Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing.
Further, the substrate pretreatment comprises the following steps in sequence:
(1.1) polishing the matrix cutter, respectively cleaning the matrix cutter with alcohol and acetone by ultrasonic waves for 8-10min, drying and fixing the matrix cutter on a sample table of a vacuum chamber;
(1.2) evacuating the vacuum chamber to at least 6.0X10 -3 Pa, heating to 200 ℃, and preserving heat for 40-120min;
(1.3) after heat preservation, the negative bias of the substrate is adjusted to 600V, argon is introduced to enable the pressure to be 0.15-0.2Pa, and plasma cleaning is carried out for 20-50min, so that the pretreated substrate is obtained.
Further, in the step (1), the thickness of the Cr transition layer is 40-60nm.
Further, in the step (2), the thickness of the CrN transition layer is 50-80nm.
Further, in the step (3), the total thickness of the NbN and NbXN nano layers is 2-3 mu m, and the tempering period is 8-10nm.
Further, in the NbXN nano-layer, X is Y, ce, la or Sc.
Further, in the step (3), the vacuum chamber pressure is maintained at 0.5 to 0.7Pa, N 2 The air flow is 20-40sccm, the total air flow is kept at 30-40%, the negative bias voltage is 200-400V, the rare earth target material opening time is 5 seconds, the interval time is 3 seconds, the Nb target sputtering power is 1500-2000W and 100kHz, the rare earth target material sputtering power is 300-500W, the quenching and tempering pulse opening time is 1 millisecond, the closing time is 1.5 milliseconds, the pulse bias voltage frequency is 100kHz, and the duty ratio is 90%.
The Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing is prepared by the preparation method of the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing.
Further, as shown in fig. 1, the matrix is sequentially provided with a Cr transition layer, a CrN transition layer and an NbN/NbXN superlattice coating from inside to outside.
In summary, the invention has the following advantages:
1. the method comprises the steps of pretreatment, heating, cleaning, preparation of a transition layer, a wear-resistant layer and the like, and adopts a direct-current unbalanced magnetron sputtering method to assist high-frequency pulse magnetron sputtering to prepare the coating. On the basis that the NbN coating has good thermal expansion coefficient, mechanical property and stability, adding rare earth elements to prepare NbN/NbXN (X is rare earth element Y, ce, la, sc) superlattice coating, utilizing the purification effect of rare earth elements on coating impurities and the promotion effect on atomic deposition efficiency and diffusion rate, and adding rare earth atoms can generate certain atomic stacking deformation energy in the coating, so that the coating has certain prestress, and the mechanical property and wear resistance of the coating can be obviously improved. Therefore, the preparation method of the invention can improve the hardness, binding force, high thermal stability, corrosion resistance and wear resistance of the coating, the coating can ensure the cutting quality and simultaneously prolong the service life, and the preparation method is simple to operate, has high production efficiency and can be widely applied to industrial production.
2. The rare earth element can purify impurity atoms in the coating; the rare earth element can improve the deposition efficiency of atoms such as Nb and the like and promote the diffusion rate of the atoms, thereby improving the binding force of the coating; the atomic radius of the rare earth elements is slightly larger than that of Nb atoms, so that certain atomic stacking deformation energy can be generated in the NbN coating, the coating has certain prestress, and the mechanical property and the wear resistance of the coating can be improved.
3. On the basis of Cr/CrN as transition layer, nbN/NbXN superlattice coating (X is rare earth element, X content is 0.1-5%) is introduced, and comprehensive performance of NbN coating is improved in all directions. The high-power pulse magnetron sputtering (HiPIMS) is adopted to deposit the multilayer superlattice coating, the peak power of the multilayer superlattice coating is 2-3 orders of magnitude higher than that of the traditional magnetron sputtering, a highly ionized sputtering material can be obtained, and the high ionization characteristic can provide more remarkable microstructure densification and surface smoothness, so that the mechanical property, the adhesion degree, the friction property and the thermal stability of the compound coating are effectively improved. The superlattice structure is utilized, the single-layer NbN/NbXN structure is controlled within 10nm, the single-layer structure nanocrystallization is realized, the toughness of the coating can be enhanced, the crack generation probability and the crack diffusion are reduced, and the overall binding force of the coating can be improved. And under the action of a proper modulation period, the hardness and the elasticity can be obviously improved.
4. By introducing a proper amount of rare earth elements into the NbN/NbXN coating and combining a superlattice coating structure, the coating performance, such as surface hardness, wear resistance, fracture toughness, fatigue strength and film base binding force (improved to 80N), can be obviously improved, and the active element effect is utilized, so that the cutter coating has good oxidation resistance and thermal stability under the severe working condition of high speed and high temperature, and still has good cutting performance at 900 ℃.
Drawings
FIG. 1 is a schematic diagram of a Cr/CrN/NbN/NbXN rare earth superlattice coating.
Detailed Description
Example 1
The preparation method of the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing sequentially comprises the following steps:
(1) Regulating the vacuum degree to 0.3Pa, introducing 50sccm of argon, maintaining the sputtering power of a Cr target at 300W, maintaining the negative bias voltage of the matrix at 100V, depositing for 10min, and depositing a Cr transition layer with the thickness of 40nm on the surface of the pretreated matrix to obtain the Cr transition layer;
(2) Introducing nitrogen, controlling the total pressure of the vacuum chamber at 0.3Pa, ar and N 2 The partial pressure ratio is 5:2, the sputtering power of the Cr target is 450W, the negative bias voltage of the matrix is kept at 150V, the deposition time is 10min, and a CrN transition layer is deposited on the Cr transition layer obtained in the step (1) and has the thickness of 70nm, so that the CrN transition layer is obtained;
(3) In Ar/N 2 Alternately depositing NbN and NbXN nano layers in atmosphere, wherein the total thickness is 2 mu m, the tempering period is 10nm, the vacuum chamber pressure is kept at 0.5Pa, and the N 2 The air flow is 40sccm, the total air flow is kept 40%, the negative bias is 300V, the rare earth target opening time is 5 seconds, the interval time is 3 seconds, the NbY alloy target (Y content is 10%) and the pure Nb target are adopted, the sputtering power of the Nb target is 1500W and 100kHz, the sputtering power of the rare earth target is 500W, the quenching and tempering pulse opening time is 1 millisecond, the closing time is 1.5 milliseconds, the pulse bias frequency is 100kHz, the duty ratio is 90%, and the rare earth target is naturally cooled to a room after depositionAnd (3) turning off the power supply and the gas source, and applying the Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing.
The substrate pretreatment comprises the following steps in sequence:
(1.1) polishing the matrix cutter, respectively cleaning the matrix cutter with alcohol and acetone by ultrasonic waves for 10min, drying and fixing the matrix cutter on a vacuum chamber sample table;
(1.2) evacuating the vacuum chamber to at least 6.0X10 -3 Pa, heating to 200 ℃, and preserving heat for 60min;
(1.3) after heat preservation, the negative bias of the substrate is adjusted to 600V, argon is introduced to enable the pressure to be 0.15Pa, and plasma cleaning is carried out for 30min, so that the pretreated substrate is obtained.
Example 2
The preparation method of the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing sequentially comprises the following steps:
(1) Regulating the vacuum degree to 0.4Pa, introducing argon gas at 60sccm, sputtering the Cr target with power of 300W, maintaining the negative bias voltage of 150V for 10min, and depositing a Cr transition layer with thickness of 50nm on the surface of the pretreated substrate to obtain a Cr transition layer;
(2) Introducing nitrogen, controlling the total pressure of the vacuum chamber to be 0.4Pa, ar and N 2 The partial pressure ratio is 5:1, the sputtering power of the Cr target is 350W, the negative bias voltage of the matrix is kept at 100V, the deposition time is 10min, and a CrN transition layer is deposited on the Cr transition layer obtained in the step (1) and has the thickness of 50nm, so that the CrN transition layer is obtained;
(3) In Ar/N 2 Alternately depositing NbN and NbXN nano layers in atmosphere, wherein the total thickness is 2.5 mu m, the tempering period is 10nm, the vacuum chamber pressure is kept at 0.6Pa, and the N 2 The gas flow is 40sccm, the total gas flow is kept 40%, the negative bias is 400V, the rare earth target opening time is 5 seconds, the interval time is 3 seconds, an NbCe alloy target (the Ce content is 10%) and a pure Nb target are adopted, the Nb target sputtering power is 1900W and 100kHz, the rare earth target sputtering power is 400W, the quenching and tempering pulse opening time is 1 millisecond, the closing time is 1.5 milliseconds, the pulse bias frequency is 100kHz, the duty ratio is 90%, the deposited rare earth target is naturally cooled to room temperature, the power supply and the gas source are closed, and the Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing is adopted.
The substrate pretreatment comprises the following steps in sequence:
(1.1) polishing the matrix cutter, respectively cleaning the matrix cutter with alcohol and acetone by ultrasonic waves for 10min, drying and fixing the matrix cutter on a vacuum chamber sample table;
(1.2) evacuating the vacuum chamber to at least 6.0X10 -3 Pa, heating to 200 ℃, and preserving heat for 40min;
(1.3) after heat preservation, the negative bias of the substrate is adjusted to 600V, argon is introduced to enable the pressure to be 0.18Pa, and plasma cleaning is carried out for 40min, so that the pretreated substrate is obtained.
Example 3
The preparation method of the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing sequentially comprises the following steps:
(1) Regulating the vacuum degree to 0.3Pa, introducing argon to 50sccm, maintaining the sputtering power of the Cr target at 350W, maintaining the negative bias voltage of the matrix at 100V, depositing for 10min, and depositing a Cr transition layer on the surface of the pretreated matrix to obtain a Cr transition layer with the thickness of 50 nm;
(2) Introducing nitrogen, controlling the total pressure of the vacuum chamber at 0.3Pa, ar and N 2 The partial pressure ratio is 5:2, the sputtering power of the Cr target is 400W, the negative bias voltage of the matrix is kept at 100V, the deposition time is 10min, and a CrN transition layer is deposited on the Cr transition layer obtained in the step (1) and has the thickness of 60nm, so that the CrN transition layer is obtained;
(3) In Ar/N 2 Alternately depositing NbN and NbXN nano layers in atmosphere, wherein the total thickness is 3 mu m, the tempering period is 10nm, the vacuum chamber pressure is kept at 0.6Pa, and the N 2 The gas flow is 40sccm, the total gas flow is kept 40%, the negative bias is 300V, the rare earth target opening time is 5 seconds, the interval time is 3 seconds, an NbLa alloy target (La content is 10%) and a pure Nb target are adopted, the Nb target sputtering power is 2000W and 100kHz, the rare earth target sputtering power is 400W, the quenching and tempering pulse opening time is 1 millisecond, the closing time is 1.5 milliseconds, the pulse bias frequency is 100kHz, the duty ratio is 90%, the deposited rare earth target is naturally cooled to room temperature, the power supply and the gas source are closed, and the Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing is adopted.
The substrate pretreatment comprises the following steps in sequence:
(1.1) polishing the matrix cutter, respectively cleaning the matrix cutter with alcohol and acetone by ultrasonic waves for 10min, drying and fixing the matrix cutter on a vacuum chamber sample table;
(1.2) evacuating the vacuum chamber to at least 6.0X10 -3 Pa, heating to 200 ℃, and preserving heat for 40min;
(1.3) after heat preservation, the negative bias of the substrate is adjusted to 600V, argon is introduced to enable the pressure to be 0.18Pa, and plasma cleaning is carried out for 50min, so that the pretreated substrate is obtained.
The Cr/CrN/NbN/NbXN rare earth superlattice coating obtained in example 1 was compared with NbBN composite coating and TiN/NbN multilayer film, and the results are shown in Table 1.
TABLE 1 comparison of properties of NbBN composite coating, tiN/NbN multilayer film and NbN/NbXN superlattice coating
As shown in Table 1, the invention introduces NbN/NbXN superlattice coating (X is rare earth element, and X content is 0.1-5%) on the basis of Cr/CrN as transition layer, and improves comprehensive performance of NbN coating in all directions.
Although specific embodiments of the invention have been described in detail with reference to the accompanying drawings, it should not be construed as limiting the scope of protection of the present patent. Various modifications and variations which may be made by those skilled in the art without the creative effort are within the scope of the patent described in the claims.
Claims (7)
1. The preparation method of the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing is characterized by sequentially comprising the following steps of:
(1) Regulating the vacuum degree to 0.25-0.4Pa, introducing argon to 40-70sccm, and keeping the sputtering power of the Cr target at 300-400W, wherein the negative bias voltage of the substrate is kept at 40-200V, the deposition time is 10-20min, and depositing a Cr transition layer on the surface of the pretreated substrate to obtain the Cr transition layer;
(2) Introducing nitrogen, controlling the total pressure of the vacuum chamber to be 0.3-0.5Pa, ar and N 2 The partial pressure ratio is 5:1-2, the sputtering power of the Cr target is 300-500W, and the substrate is negatively biasedKeeping the temperature at 40-200V, and depositing for 10-20min, and depositing a CrN transition layer on the Cr transition layer obtained in the step (1) to obtain the CrN transition layer;
(3) In Ar/N 2 Alternately depositing NbN and NbXN nano layers in the atmosphere, naturally cooling to room temperature after deposition, and turning off a power supply and a gas source to obtain the Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing;
wherein, in the NbXN nano layer, X is Y, ce, la or Sc;
in step (3), the vacuum chamber pressure is maintained at 0.5-0.7Pa, N 2 The air flow is 20-40sccm, the total air flow is kept at 30-40%, the negative bias voltage is 200-400V, the rare earth target material opening time is 5 seconds, the interval time is 3 seconds, the Nb target sputtering power is 1500-2000W and 100kHz, the rare earth target material sputtering power is 300-500W, the quenching and tempering pulse opening time is 1 millisecond, the closing time is 1.5 milliseconds, the pulse bias voltage frequency is 100kHz, and the duty ratio is 90%.
2. The method for preparing a Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing according to claim 1, wherein the substrate pretreatment comprises the following steps in order:
(1.1) polishing the matrix cutter, respectively cleaning the matrix cutter with alcohol and acetone by ultrasonic waves for 8-10min, drying and fixing the matrix cutter on a sample table of a vacuum chamber;
(1.2) evacuating the vacuum chamber to at least 6.0X10 -3 Pa, heating to 200 ℃, and preserving heat for 40-120min;
(1.3) after heat preservation, the negative bias of the substrate is adjusted to 600V, argon is introduced to enable the pressure to be 0.15-0.2Pa, and plasma cleaning is carried out for 20-50min, so that the pretreated substrate is obtained.
3. The method for producing a Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing according to claim 1, wherein in step (1), the Cr transition layer thickness is 40-60nm.
4. The method for preparing a Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing according to claim 1, wherein in step (2), the CrN transition layer thickness is 50-80nm.
5. The method for preparing a Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing according to claim 1, wherein in step (3), the total thickness of the alternately deposited NbN and NbXN nanolayers is 2-3 μm, and the tempering period is 8-10nm.
6. A Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing produced by the method of producing a Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing as defined in any of claims 1-5.
7. The Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing according to claim 6, wherein the Cr transition layer, crN transition layer, and NbN/NbXN superlattice coating are sequentially present from the inside to the outside of the substrate.
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| CN104321460A (en) * | 2012-05-02 | 2015-01-28 | 韩国冶金株式会社 | Hard coating for cutting tool |
| CN109686838A (en) * | 2017-10-18 | 2019-04-26 | 旺宏电子股份有限公司 | Class superlattices (SUPERLATTICE-LIKE) switch element |
| CN210287481U (en) * | 2019-04-11 | 2020-04-10 | 深圳南科超膜材料技术有限公司 | Cutter coating for die steel processing |
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| US5783295A (en) * | 1992-11-09 | 1998-07-21 | Northwestern University | Polycrystalline supperlattice coated substrate and method/apparatus for making same |
| JP3813740B2 (en) * | 1997-07-11 | 2006-08-23 | Ｔｄｋ株式会社 | Substrates for electronic devices |
| CH701726B1 (en) * | 2010-05-11 | 2011-03-15 | Medacta Int Sa | Metal substrate comprises nitride-based ceramic coatings used for the production of the joints of orthopedic implants |
| JP5640242B2 (en) * | 2011-02-01 | 2014-12-17 | 住友電工ハードメタル株式会社 | Surface coated cutting tool |
| CN109962134B (en) * | 2019-04-10 | 2022-02-18 | 福建省南安市清信石材有限公司 | Nitride semiconductor light-emitting diode |
| CN111969099A (en) * | 2020-08-26 | 2020-11-20 | 中国科学院上海微系统与信息技术研究所 | Stack structure SNS Josephson junction, voltage reference and preparation method |
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| CN104321460A (en) * | 2012-05-02 | 2015-01-28 | 韩国冶金株式会社 | Hard coating for cutting tool |
| CN109686838A (en) * | 2017-10-18 | 2019-04-26 | 旺宏电子股份有限公司 | Class superlattices (SUPERLATTICE-LIKE) switch element |
| CN210287481U (en) * | 2019-04-11 | 2020-04-10 | 深圳南科超膜材料技术有限公司 | Cutter coating for die steel processing |
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