CN114059029A - 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, wherein the preparation method sequentially comprises the following steps: (1) adjusting the vacuum degree, introducing argon, and depositing a Cr transition layer on the surface of the matrix after pretreatment to obtain a 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 high-temperature alloy 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, ensures the cutting quality and prolongs the service life.
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 and manufacturing industry, the demand of industrial production for high-temperature alloys with excellent comprehensive properties is increased sharply, but the difficulty in processing is a great difficulty faced by the high-temperature alloys. In the face of this dilemma, cemented carbide tool coatings also develop towards high hardness, good chemical stability, high temperature oxidation resistance, and excellent high temperature thermal stability. The coating composition and structure are updated, the element composition begins to diversify, the number of coating layers begins to increase, and the microstructure tends to be nano-sized from a columnar crystal structure. The common binary and ternary coatings comprise three types of nitrides, carbides and oxides, the nitride based TiAlN is mainly used at present, but when materials which are difficult to process such as high-temperature alloy and the like are processed, the defects of low hardness, high wear rate, poor oxidation resistance and the like are difficult to meet the requirements of the processing industry.
The NbN coating firstly enters the visual field because of the ultrahigh superconducting critical transition temperature, the excellent mechanical property of the NbN becomes the key point of the research with the research, the NbN film deposited on a cutter by ion beam assisted deposition and magnetron sputtering has the hardness of more than 30Gpa and the friction coefficient of less than 0.5. In addition, the NbN-related nano multilayer film 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-multilayer films with good mechanical properties and chemical stability have attracted much attention in industrial production. The TiN/NbN nano multilayer film mainly comprises two phases of face-centered cubic NbN and face-centered cubic TiN, utilizes an excellent periodic layered structure, has the hardness of 40GPa and the elastic modulus of 465GPa, but has poor integral wear resistance and friction coefficient of more than 0.5, and can generate wear-through phenomenon in long-term cutting. Although some researchers invented the NbBN composite coating, the wear rate is reduced, but the microhardness is only 31 GPa; the elastic modulus drops to 366GPa, which is a severe 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, so that the hardness, the bonding force, the high thermal stability, the corrosion resistance and the wear resistance of the coating are improved, the cutting quality is ensured, and the service life is prolonged.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: provides a preparation method of Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing, which comprises the following steps in sequence:
(1) adjusting the vacuum degree to 0.25-0.4Pa, introducing argon gas to 40-70sccm, sputtering the Cr target with the power of 300-400W, keeping the negative bias voltage of the substrate at 40-200V, depositing for 10-20min, and depositing a Cr transition layer on the surface of the substrate after the pretreatment to obtain the Cr transition layer;
(2) introducing nitrogen, controlling the total pressure of the vacuum chamber at 0.3-0.5Pa, Ar and N2The partial pressure ratio is 5:1-2, the sputtering power of the Cr target is 300-;
(3) at Ar/N2Alternately 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 high-temperature alloy processing.
Further, the pretreatment of the matrix sequentially comprises the following steps:
(1.1) polishing the base cutter, ultrasonically cleaning for 8-10min by using alcohol and acetone respectively, drying and fixing on a sample table in a vacuum chamber;
(1.2) evacuating the vacuum chamber to at least 6.0X 10-3Pa, heating to 200 ℃, and keeping the temperature for 40-120 min;
(1.3) keeping the temperature, adjusting the negative bias of the substrate to 600V, introducing argon to enable the pressure to be 0.15-0.2Pa, and cleaning the substrate for 20-50min by using plasma to obtain the pretreated substrate.
Furthermore, in the step (1), the thickness of the Cr transition layer is 40-60 nm.
Further, in the step (2), the thickness of the CrN transition layer is 50-80 nm.
Furthermore, in the step (3), the total thickness of the alternately deposited NbN and NbXN nanolayers is 2-3 μm, and the quenching and tempering period is 8-10 nm.
Further, in the NbXN nanolayer, X is Y, Ce, La or Sc.
Further, in the step (3), the pressure of the vacuum chamber is kept between 0.5 and 0.7Pa, N2The gas flow is 20-40sccm, the gas flow is kept at 30-40% of the total gas flow, the negative bias voltage is 200-400V, the rare earth target is opened for 5 seconds and is spaced for 3 seconds, the Nb target sputtering power is 1500-2000W and 100kHz, the rare earth target sputtering power is 300-500W, the quenching and tempering pulse is opened for 1 millisecond and is closed for 1.5 milliseconds, the pulse bias 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, a Cr transition layer, a CrN transition layer and an NbN/NbXN superlattice coating are sequentially arranged from the inside to the outside of the substrate.
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 the preparation of the coating is carried out by adopting a direct-current unbalanced magnetron sputtering method to assist high-frequency pulse magnetron sputtering. On the basis that the NbN coating has good thermal expansion coefficient, mechanical property and stability, the rare earth element is added to prepare the NbN/NbXN (X is the rare earth element Y, Ce, La and Sc) superlattice coating, the rare earth element is utilized to purify the impurities of the coating and promote the atomic deposition efficiency and diffusion rate, and the addition of the rare earth element can generate certain atomic accumulation distortion energy in the coating, so that the coating has certain prestress, and the mechanical property and the wear resistance of the coating can be obviously improved. Therefore, the preparation method of the invention can improve the hardness, the bonding force, the high thermal stability, the corrosion resistance and the wear resistance of the coating, the coating can ensure the cutting quality and simultaneously improve the service life, and the preparation method has simple operation and high production efficiency, and can be widely applied to industrial production.
2. The rare earth elements can purify impurity atoms in the coating; the rare earth elements can improve the deposition efficiency of Nb and other atoms 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, and certain atom accumulation distortion energy can be generated in the NbN coating, so that the coating has certain prestress, and the mechanical property and the wear resistance of the coating can be improved.
3. The NbN/NbXN superlattice coating (X is rare earth element, and the content of X is 0.1-5%) is introduced on the basis of taking Cr/CrN as a transition layer, and the comprehensive performance of the NbN coating is improved in an all-round way. The high-power pulse magnetron sputtering (HiPIMS) is adopted to deposit the multi-layer superlattice coating, the peak power of the coating is 2-3 orders of magnitude higher than that of the conventional 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 performance of the coating can be obviously improved, such as the surface hardness, the wear resistance, the fracture toughness, the fatigue strength and the film-substrate binding force (improved to 80N) are improved, and the effect of active elements is utilized, so that the cutter coating has good oxidation resistance and thermal stability under the severe working conditions of high speed and high temperature, and still has good cutting performance at 900 ℃.
Drawings
FIG. 1 is a schematic diagram of the structure of Cr/CrN/NbN/NbXN rare earth superlattice coating.
Detailed Description
Example 1
A Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing is prepared by the following steps in sequence:
(1) adjusting the vacuum degree to 0.3Pa, introducing argon gas of 50sccm, sputtering the Cr target with the power of 300W, keeping the negative bias voltage of the substrate at 100V, depositing for 10min, and depositing a Cr transition layer with the thickness of 40nm on the surface of the substrate after the pretreatment to obtain the Cr transition layer;
(2) introducing nitrogen, controlling the total pressure of the vacuum chamber to be 0.3Pa, Ar and N2The partial pressure ratio is 5:2, the sputtering power of the Cr target is 450W, the negative bias of the matrix is kept at 150V, the deposition time is 10min, a CrN transition layer is deposited on the Cr transition layer obtained in the step (1), and the thickness is 70nm, so that the CrN transition layer is obtained;
(3) at Ar/N2Alternately depositing NbN and NbXN nanolayers in an atmosphere with a total thickness of 2 μm, a hardening and tempering period of 10nm, and a vacuum chamber pressure of 0.5Pa, N2The gas flow is 40sccm, the gas flow is kept to be 40% of the total gas flow, the negative bias is 300V, the rare earth target opening time is 5 seconds, the interval time is 3 seconds, NbY alloy target (Y content is 10%) and pure Nb target are adopted, the Nb target sputtering power is 1500W and 100kHz, the rare earth target sputtering power 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%, the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing is obtained by naturally cooling to the room temperature after deposition and closing a power supply and a gas source.
The pretreatment of the matrix sequentially comprises the following steps:
(1.1) polishing the base cutter, ultrasonically cleaning for 10min by using alcohol and acetone respectively, drying and fixing on a sample table in a vacuum chamber;
(1.2) evacuating the vacuum chamber to at least 6.0X 10-3Pa, heating to 200 ℃, and keeping the temperature for 60 min;
(1.3) regulating the negative bias of the substrate to 600V after heat preservation, introducing argon to enable the pressure to be 0.15Pa, and cleaning the substrate for 30min by using plasma to obtain the pretreated substrate.
Example 2
A Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing is prepared by the following steps in sequence:
(1) adjusting the vacuum degree to 0.4Pa, introducing argon gas of 60sccm, sputtering the Cr target with the power of 300W, keeping the negative bias voltage of the substrate at 150V, depositing for 10min, and depositing a Cr transition layer with the thickness of 50nm on the surface of the substrate after the pretreatment to obtain the Cr transition layer;
(2) introducing nitrogen, controlling the total pressure of the vacuum chamber to be 0.4Pa, Ar and N2The partial pressure ratio is 5:1, the sputtering power of the Cr target is 350W, the negative bias of the matrix is kept at 100V, the deposition time is 10min, a CrN transition layer is deposited on the Cr transition layer obtained in the step (1), and the thickness of the CrN transition layer is 50nm to obtain a CrN transition layer;
(3) at Ar/N2Alternately depositing NbN and NbXN nanolayers in an atmosphere with a total thickness of 2.5 μm, a hardening and tempering period of 10nm, and a vacuum chamber pressure of 0.6Pa, N2The gas flow is 40sccm, the gas flow is kept to be 40% of the total gas flow, 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 deposition is naturally cooled to the room temperature, and the power supply and the gas source are closed, so that the Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing is obtained.
The pretreatment of the matrix sequentially comprises the following steps:
(1.1) polishing the base cutter, ultrasonically cleaning for 10min by using alcohol and acetone respectively, drying and fixing on a sample table in a vacuum chamber;
(1.2) evacuating the vacuum chamber to at least 6.0X 10-3Pa, heating to 200 ℃, and keeping the temperature for 40 min;
(1.3) keeping the temperature, adjusting the negative bias of the substrate to 600V, introducing argon to enable the pressure to be 0.18Pa, and cleaning the substrate for 40min by plasma to obtain the pretreated substrate.
Example 3
A Cr/CrN/NbN/NbXN rare earth superlattice coating for high-temperature alloy processing is prepared by the following steps in sequence:
(1) adjusting the vacuum degree to 0.3Pa, introducing argon gas of 50sccm, sputtering the Cr target with the power of 350W, keeping the negative bias voltage of the substrate at 100V, depositing for 10min, and depositing a Cr transition layer with the thickness of 50nm on the surface of the substrate after the pretreatment to obtain the Cr transition layer;
(2) introducing nitrogen, controlling the total pressure of the vacuum chamber to be 0.3Pa, Ar and N2The partial pressure ratio is 5:2, the sputtering power of the Cr target is 400W, the negative bias of the matrix is kept at 100V, the deposition time is 10min, a CrN transition layer is deposited on the Cr transition layer obtained in the step (1), and the thickness is 60nm, so that the CrN transition layer is obtained;
(3) at Ar/N2Alternately depositing NbN and NbXN nanolayers in an atmosphere with a total thickness of 3 μm, a hardening and tempering period of 10nm, and a vacuum chamber pressure of 0.6Pa, N2The gas flow is 40sccm, the gas flow is kept to be 40% of the total gas flow, the negative bias is 300V, the rare earth target opening time is 5 seconds, the interval time is 3 seconds, a NbLa alloy target (the 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 Cr/CrN/NbN/NbXN rare earth superlattice coating for processing the high-temperature alloy is obtained by naturally cooling to the room temperature after deposition and closing a power supply and a gas source.
The pretreatment of the matrix sequentially comprises the following steps:
(1.1) polishing the base cutter, ultrasonically cleaning for 10min by using alcohol and acetone respectively, drying and fixing on a sample table in a vacuum chamber;
(1.2) evacuating the vacuum chamber to at least 6.0X 10-3Pa, heating to 200 ℃, and keeping the temperature for 40 min;
(1.3) keeping the temperature, adjusting the negative bias of the substrate to 600V, introducing argon to enable the pressure to be 0.18Pa, and cleaning the substrate for 50min by using plasma to obtain the pretreated substrate.
The Cr/CrN/NbN/NbXN rare earth superlattice coating obtained in the example 1 is compared with the NbBN composite coating and the TiN/NbN multilayer film in performance, and the result is shown in a table 1.
TABLE 1 comparison of NbBN composite coatings, TiN/NbN multilayer films, and NbN/NbXN superlattice coatings
As can be seen from Table 1, the NbN/NbXN superlattice coating (X is a rare earth element, and the content of X is 0.1-5%) is introduced on the basis of taking Cr/CrN as a transition layer, so that the comprehensive performance of the NbN coating is improved in an all-round manner.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (9)
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) adjusting the vacuum degree to 0.25-0.4Pa, introducing argon gas to 40-70sccm, sputtering the Cr target with the power of 300-400W, keeping the negative bias voltage of the substrate at 40-200V, depositing for 10-20min, and depositing a Cr transition layer on the surface of the substrate after the pretreatment to obtain the Cr transition layer;
(2) introducing nitrogen, controlling the total pressure of the vacuum chamber at 0.3-0.5Pa, Ar and N2The partial pressure ratio is 5:1-2, the sputtering power of the Cr target is 300-;
(3) at Ar/N2Alternately 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 high-temperature alloy processing.
2. The method of claim 1, wherein the pre-treatment of the substrate comprises the following steps in sequence:
(1.1) polishing the base cutter, ultrasonically cleaning for 8-10min by using alcohol and acetone respectively, drying and fixing on a sample table in a vacuum chamber;
(1.2) evacuating the vacuum chamber to at least 6.0X 10-3Pa, heating to 200 ℃, and keeping the temperature for 40-120 min;
(1.3) keeping the temperature, adjusting the negative bias of the substrate to 600V, introducing argon to enable the pressure to be 0.15-0.2Pa, and cleaning the substrate for 20-50min by using plasma to obtain the pretreated substrate.
3. The method of claim 1, wherein in step (1), the thickness of the Cr transition layer is 40-60 nm.
4. The method of claim 1, wherein in step (2), the CrN transition layer has a thickness of 50-80 nm.
5. The method of claim 1, wherein the total thickness of the alternately deposited NbN and NbXN nanolayers in step (3) is 2-3 μm, and the thermal refining period is 8-10 nm.
6. The method of claim 1, wherein in the NbXN nanolayer, X is Y, Ce, La, or Sc.
7. The method of claim 1, wherein in step (3), the pressure in the vacuum chamber is maintained at 0.5-0.7Pa, and the pressure in the vacuum chamber is maintained at N2The gas flow is 20-40sccm, the gas flow is kept at 30-40% of the total gas flow, the negative bias voltage is 200-400V, the rare earth target is opened for 5 seconds and is spaced for 3 seconds, the Nb target sputtering power is 1500-2000W and 100kHz, the rare earth target sputtering power is 300-500W, the quenching and tempering pulse is opened for 1 millisecond and is closed for 1.5 milliseconds, the pulse bias frequency is 100kHz, and the duty ratio is 90%.
8. The Cr/CrN/NbN/NbXN rare earth superlattice coating for high temperature alloy processing prepared by the preparation method of the Cr/CrN/NbN/NbXN rare earth superlattice coating for high temperature alloy processing as claimed in any one of claims 1-7.
9. The Cr/CrN/NbN/NbXN rare earth superlattice coating for superalloy processing as claimed in claim 8, wherein the Cr transition layer, the CrN transition layer and the NbN/NbXN superlattice coating are arranged from the substrate from the inside to the outside.
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| CN115233171B (en) * | 2022-06-23 | 2023-06-20 | 贵州大学 | High-entropy superlattice nitride coating and preparation method thereof |
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| CN114059029B (en) | 2023-05-09 |
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