Nickel-based interface cone coating, nickel-based interface cone and preparation method

Abstract

The invention relates to a nickel-based interface cone coating, a nickel-based interface cone and a preparation method, the coating is a multi-layer boride coating, the multi-layer boride coating comprises a nickel boride layer, an other metal boride layer and a lanthanum hexaboride layer, the nickel boride layer is the innermost layer, and the lanthanum hexaboride layer is the outermost layer. Multiple boride coatings are prepared on the surface of the nickel-based interface cone through the vacuum magnetron sputtering technology, the nickel boride coating is arranged on the innermost side, the nickel boride can form a coating which is tightly combined and high in strength with the nickel-based interface cone, the middle coating is other metal boride coatings, the hardness, the strength and the heat conduction performance are high, and the nickel-based interface cone has the good heat conduction performance. According to the present invention, the lanthanum hexaboride coating is used as the outer layer, and can provide the supporting effect on the boride multilayer film, the outermost layer is the lanthanum hexaboride coating, the lanthanum hexaboride has good chemical stability, the introduction of other impurity atoms during the detection process is reduced, and the preparation cost of the coating is reduced by 10-20% compared with the platinum group metal coating.

Description

Technical Field

[0001] The invention relates to the technical field of inductively coupled plasma mass spectrometers, and in particular to a nickel-based interface cone coating, a nickel-based interface cone and a preparation method thereof. Background Art

[0002] In modern analytical science, inductively coupled plasma mass spectrometer (ICP-MS) is a high-precision element detection and analysis instrument with the advantages of high efficiency and accuracy, simultaneous analysis of multiple elements, isotope analysis, high sensitivity and low detection limit. It is an indispensable emerging trace analysis technology. The instrument usually uses an interface cone structure to connect the inductively coupled plasma source and the mass spectrometer. The transmission characteristics of the interface cone directly affect the analytical performance of the instrument. The interface cone needs to withstand high temperature, high pressure and corrosive environment during work, so the interface cone needs to have good heat resistance, corrosion resistance and thermal conductivity. In order to extend the service life of the interface cone, a coating is usually prepared on the surface of the nickel-based interface cone to protect the nickel-based interface cone. The common coatings currently include oxide ceramic coatings and platinum group metal coatings. The thermal conductivity of the ceramic coating is poor, which affects the heat dissipation of the nickel-based interface cone. At the same time, the ceramic material has poor acid corrosion resistance, which affects the use environment and life of the interface cone; although the platinum group metal coating has good thermal conductivity and corrosion resistance, its use cost is high, which greatly increases the cost of a single test. Summary of the invention

[0003] In view of the problems in the above-mentioned prior art that the nickel-based interface cone has a short service life when coated with an oxide ceramic coating, is restricted in the use environment, and has a high detection cost when coated with a platinum group metal coating, the present invention provides a nickel-based interface cone coating, a nickel-based interface cone and a preparation method.

[0004] To achieve the above object, the technical solution of the present invention is as follows:

[0005] A nickel-based interface cone coating, which is a multi-layer boride coating, comprising a nickel boride layer, other metal boride layers and a lanthanum hexaboride layer, wherein the nickel boride layer is the innermost layer, the lanthanum hexaboride layer is the outermost layer, and the other metal boride layers include one or more elements of tantalum, tungsten, zirconium, molybdenum, titanium and cerium.

[0006] Furthermore, the coating has a thickness of 0.3-0.5 μm, and / or a density of ≥99.8%, and / or a purity of ≥99.99%, and / or a grain size of ≤1 μm, and / or a surface roughness of <0.5 μm.

[0007] Furthermore, the thermal conductivity of the coating is ≥110 W / m·K, and / or the coating can withstand plasma bombardment of 4000-8000 K, and / or the coating can work continuously for ≥56 h, and / or the service life of the coating is 12-24 months, and / or the coating can withstand corrosion in an acid-base environment with a pH of ≤3 and a pH of ≥9, and the corrosion products do not fall off, and the corrosion products introduced during detection are ≤0.5 ppm.

[0008] The present invention also includes the following technical solutions:

[0009] A nickel-based interface cone with the coating.

[0010] The present invention also includes the following technical solutions:

[0011] A method for preparing the nickel-based interface cone with a coating comprises the following steps:

[0012] (1) Pre-sputtering: The nickel-based interface cone is placed in the magnetron sputtering chamber. The magnetron sputtering chamber is inert atmosphere and the pressure is maintained at 1×10 -1 -3×10 -1 Pa; close the sputtering baffle, and sputter nickel boride, one or more other metal borides and lanthanum hexaboride targets one by one, with a sputtering power of 30-150W and a sputtering time of 3-15min;

[0013] (2) Sputtering coating: Heat the nickel-based interface cone to 100-250°C and keep it for 5-15 minutes. The magnetron sputtering chamber is inert atmosphere and the pressure is maintained at 2×10 -1 -5×10 -1 Pa; open the sputtering baffle, and sputter the nickel boride coating, one or more other metal boride coatings and the lanthanum hexaboride coating in sequence, the sputtering power is 40-80W, the sputtering time of each coating layer is 2-8min, and the total sputtering time is ≤14min;

[0014] (3) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 200-500℃ and keep it for 0.5-3h, then cool it for 5-8h and take out the interface cone.

[0015] Furthermore, before pre-sputtering, the nickel-based interface cone is immersed in a mixed solution of hydrochloric acid: sulfuric acid with a volume ratio of 1:0.9-1.2 for 5-15 minutes and then dried for 10-30 minutes, wherein the concentrations of the hydrochloric acid and the sulfuric acid are both ≤10%.

[0016] Furthermore, the sputtering power supply is an alternating current power supply.

[0017] Furthermore, the boride target material described in step (1) and step (2) is a boride of one element selected from the group consisting of nickel, lanthanum, tantalum, tungsten, zirconium, molybdenum, titanium and cerium, and the purity of the boride target material is ≥99.99% and the grain size is ≤20 μm.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] The invention provides a nickel-based interface cone coating, a nickel-based interface cone and a preparation method. A multilayer boride coating is prepared on the surface of the nickel-based interface cone by a vacuum magnetron sputtering process, wherein the innermost layer is a nickel boride coating, which can form a coating with a tight bond and high strength with the nickel-based interface cone, the middle coating is other metal boride coatings, which have high hardness, strength and thermal conductivity, and can provide support for the boride multilayer film, and the outermost layer is a lanthanum hexaboride coating, which has good chemical stability and reduces the introduction of other impurity atoms during the detection process. Compared with the platinum group metal coating, the coating saves 10%-20% of the preparation cost. The nickel-based interface cone coated with the coating can withstand the bombardment of high-temperature plasma of 4000-8000K, can work continuously for ≥56h, and has a service life of 12-24 months; the nickel-based interface cone coated with the coating can also withstand acid-base environment corrosion of pH≤3 and pH≥9, and the corrosion products do not fall off, and the introduction of corrosion products is ≤0.5ppm during detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The embodiments of the present invention are further described below with reference to the accompanying drawings, in which:

[0021] Figure 1 A schematic diagram of multi-layer boride coating is shown;

[0022] Description of the drawings: 1-lanthanum hexaboride coating, 2-other metal boride coating, 3-nickel boride coating. DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below through specific embodiments in conjunction with the accompanying drawings. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0024] Example 1

[0025] A method for preparing a nickel-based interface cone with a coating comprises the following steps:

[0026] (1) Pretreatment: Soak the interface cone in the cleaning solution for 5 minutes and dry it for 20 minutes;

[0027] (2) Pre-sputtering: Place the nickel-based interface cone into the magnetron sputtering chamber, evacuate the chamber, and introduce inert gas into the chamber to maintain the pressure in the chamber at 2.5×10 -1 Pa; close the sputtering baffle, and sputter nickel boride, molybdenum boride, tantalum boride and lanthanum hexaboride targets one by one, with a sputtering power of 65W and a sputtering time of 8min;

[0028] (3) Sputtering coating: The nickel-based interface cone was heated to 200 °C and maintained for 14 min. The magnetron sputtering chamber was inert atmosphere and the pressure was maintained at 4 × 10 -1 Pa; open the sputtering baffle, turn on the magnetron sputtering power supply of the nickel boride target, adjust the power to 40W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the molybdenum boride target, adjust the power to 50W, the sputtering time to 4min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the tantalum boride target, adjust the power to 80W, the sputtering time to 5min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the lanthanum hexaboride target, adjust the power to 60W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion;

[0029] (4) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 200℃ and keep it for 3h, then take out the interface cone after cooling for 6h.

[0030] It has been tested that the nickel-based interface cone with a multi-layer boride coating can withstand high-temperature plasma bombardment of 4000-8000K, can work continuously for ≥56h, has a service life of 24 months, can withstand corrosion in acidic and alkaline environments with pH≤3 and pH≥9, and the corrosion products do not fall off. During the test, the introduction of corrosion products is ≤0.5ppm; the prepared coating thickness is 0.5μm, the density is ≥99.8%, the purity is ≥99.99%, the grain size is ≤1μm, the surface roughness is <0.5μm, and the thermal conductivity is ≥115W / m·K.

[0031] Example 2

[0032] A method for preparing a nickel-based interface cone with a coating comprises the following steps:

[0033] (1) Pretreatment: Soak the interface cone in the cleaning solution for 15 minutes and dry it for 30 minutes;

[0034] (2) Pre-sputtering: Place the nickel-based interface cone into the magnetron sputtering chamber, evacuate the chamber, and introduce inert gas into the chamber to maintain the pressure in the chamber at 3×10 -1Pa; close the sputtering baffle, and sputter nickel boride, tungsten boride, tantalum boride, cerium boride and lanthanum hexaboride targets one by one, with a sputtering power of 150W and a sputtering time of 3min;

[0035] (3) Sputtering coating: The nickel-based interface cone was heated to 100 °C and maintained for 15 min. The magnetron sputtering chamber was inert atmosphere and the pressure was maintained at 2 × 10 -1 Pa; open the sputtering baffle, turn on the magnetron sputtering power supply of the nickel boride target, adjust the power to 40W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the cerium boride target, adjust the power to 45W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the tungsten boride target, adjust the power to 65W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the tantalum boride target, adjust the power to 65W, the sputtering time to 5min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the lanthanum hexaboride target, adjust the power to 60W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion;

[0036] (4) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 500℃ and keep it for 0.5h. Then take out the interface cone after cooling for 8h.

[0037] It has been tested that the nickel-based interface cone with a multi-layer boride coating can withstand high-temperature plasma bombardment of 4000-8000K, can work continuously for ≥56h, has a service life of 12 months, can withstand corrosion in acidic and alkaline environments with pH≤3 and pH≥9, and the corrosion products do not fall off. During the test, the introduction of corrosion products is ≤0.5ppm; the prepared coating thickness is 0.4μm, the density is ≥99.8%, the purity is ≥99.99%, the grain size is ≤1μm, the surface roughness is <0.5μm, and the thermal conductivity is ≥110W / m·K.

[0038] Example 3

[0039] A method for preparing a nickel-based interface cone with a coating comprises the following steps:

[0040] (1) Pretreatment: Soak the interface cone in the cleaning solution for 10 minutes and dry it for 10 minutes;

[0041] (2) Pre-sputtering: Place the nickel-based interface cone into the magnetron sputtering chamber, evacuate the chamber, and introduce inert gas into the chamber to maintain the pressure in the chamber at 1×10 -1 Pa; close the sputtering baffle, and sputter nickel boride, titanium boride, zirconium boride, tantalum boride and lanthanum hexaboride targets one by one, with a sputtering power of 30 W and a sputtering time of 15 min;

[0042] (3) Sputtering coating: The nickel-based interface cone was heated to 250 °C and maintained for 5 min. The magnetron sputtering chamber was inert atmosphere and the pressure was maintained at 5 × 10 -1 Pa; open the sputtering baffle, turn on the magnetron sputtering power supply of the nickel boride target, adjust the power to 40W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the titanium boride target, adjust the power to 50W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the zirconium boride target, adjust the power to 65W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the tantalum boride target, adjust the power to 80W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the lanthanum hexaboride target, adjust the power to 60W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion;

[0043] (4) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 350℃ and keep it for 2h, then take out the interface cone after cooling for 6.5h.

[0044] It has been tested that the nickel-based interface cone with a multi-layer boride coating can withstand high-temperature plasma bombardment of 4000-8000K, can work continuously for ≥56h, has a service life of 12 months, can withstand corrosion in acidic and alkaline environments with pH≤3 and pH≥9, and the corrosion products do not fall off. During the test, the introduction of corrosion products is ≤0.5ppm; the prepared coating thickness is 0.3μm, the density is ≥99.8%, the purity is ≥99.99%, the grain size is ≤1μm, the surface roughness is <0.5μm, and the thermal conductivity is ≥110W / m·K.

[0045] Comparative Example 1

[0046] A method for preparing a nickel-based interface cone with a coating comprises the following steps:

[0047] (1) Pretreatment: Soak the interface cone in the cleaning solution for 10 minutes and dry it for 10 minutes;

[0048] (2) Sputtering coating: The nickel-based interface cone was heated to 250°C and maintained for 5 min. The magnetron sputtering chamber was inert atmosphere and the pressure was maintained at 5×10 -1Pa; open the sputtering baffle, turn on the magnetron sputtering power supply of the nickel boride target, adjust the power to 40W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the titanium boride target, adjust the power to 50W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the zirconium boride target, adjust the power to 65W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the tantalum boride target, adjust the power to 80W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the lanthanum hexaboride target, adjust the power to 60W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion;

[0049] (3) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 350℃ and keep it for 2h, then take out the interface cone after cooling for 6.5h.

[0050] It has been tested that the nickel-based interface cone with multi-layer boride coating can withstand the high-temperature plasma bombardment of 4000-8000K, can work continuously for ≥56h, has a service life of 12 months, and can withstand acid-base corrosion in pH≤3 and pH≥9, but the corrosion products will fall off, and the corrosion products introduced during the test are ≤15ppm; the prepared coating thickness is 0.8μm, the density is ≥98%, the purity is ≥99%, the grain size is ≤5μm, the surface roughness is <3μm, and the thermal conductivity is ≥85W / m·K. This comparative example cancels the pre-sputtering process, which seriously affects the thermal conductivity and corrosion resistance of the coating, and its uneven film layer causes the corrosion products to fall off, and more impurities are introduced during the test.

[0051] Comparative Example 2

[0052] A method for preparing a nickel-based interface cone with a coating comprises the following steps:

[0053] (1) Pretreatment: Soak the interface cone in the cleaning solution for 10 minutes and dry it for 10 minutes;

[0054] (2) Pre-sputtering: Place the nickel-based interface cone into the magnetron sputtering chamber, evacuate the chamber, and introduce inert gas into the chamber to maintain the pressure in the chamber at 1×10 -1 Pa; close the sputtering baffle, sputter nickel boride and lanthanum hexaboride targets one by one, the sputtering power is 30W, and the sputtering time is 15min;

[0055] (3) Sputtering coating: The nickel-based interface cone was heated to 250 °C and maintained for 5 min. The magnetron sputtering chamber was inert atmosphere and the pressure was maintained at 5 × 10 -1Pa; open the sputtering baffle, turn on the magnetron sputtering power supply of the nickel boride target, adjust the power to 40W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the lanthanum hexaboride target, adjust the power to 60W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion;

[0056] (4) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 350℃ and keep it for 2h, then take out the interface cone after cooling for 6.5h.

[0057] The nickel-based interface cone with multi-layer boride coating can withstand the high-temperature plasma bombardment of 4000-8000K, can work continuously for ≥20h, has a service life of 6 months, can withstand acid-base environment corrosion of pH≤3 and pH≥9, and the corrosion products do not fall off. The corrosion product introduction during the test is ≤0.5ppm; the prepared coating thickness is 0.3μm, the density is ≥99.8%, the purity is ≥99.99%, the grain size is ≤1μm, the surface roughness is <0.5μm, and the thermal conductivity is ≥80W / m·K. In this comparative example, other metal boride coatings are eliminated, the hardness and strength of the coating are reduced, and the service life and thermal conductivity of the coating are seriously affected.

[0058] Comparative Example 3

[0059] A method for preparing a nickel-based interface cone with a coating comprises the following steps:

[0060] (1) Pretreatment: Soak the interface cone in the cleaning solution for 10 minutes and dry it for 10 minutes;

[0061] (2) Pre-sputtering: Place the nickel-based interface cone into the magnetron sputtering chamber, evacuate the chamber, and introduce inert gas into the chamber to maintain the pressure in the chamber at 1×10 -1 Pa; close the sputtering baffle, and sputter nickel boride, titanium boride, zirconium boride, tantalum boride and lanthanum hexaboride targets one by one, with a sputtering power of 30 W and a sputtering time of 15 min;

[0062] (3) Sputtering coating: The nickel-based interface cone was heated to 250 °C and maintained for 5 min. The magnetron sputtering chamber was inert atmosphere and the pressure was maintained at 5 × 10 -1Pa; open the sputtering baffle, turn on the magnetron sputtering power supply of the nickel boride target, adjust the power to 40W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the lanthanum hexaboride target, adjust the power to 60W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the titanium boride target, adjust the power to 50W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the zirconium boride target, adjust the power to 65W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the tantalum boride target, adjust the power to 80W, the sputtering time to 2min, and turn off the magnetron sputtering power supply after completion;

[0063] (4) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 350℃ and keep it for 2h, then take out the interface cone after cooling for 6.5h.

[0064] It has been tested that the nickel-based interface cone with multi-layer boride coating can withstand the high-temperature plasma bombardment of 4000-8000K, can work continuously for ≥56h, has a service life of 12 months, and can withstand acid-base corrosion in pH≤3 and pH≥9, but the corrosion products will fall off, and the corrosion products introduced during the test are ≤15ppm; the prepared coating thickness is 0.3μm, the density is ≥98%, the purity is ≥99%, the grain size is ≤5μm, the surface roughness is <3μm, and the thermal conductivity is ≥110W / m·K. In this comparative example, the lanthanum hexaboride layer is used as the middle layer and the other metal boride layer is used as the outermost layer. The chemical stability of the other metal boride layer is poor relative to the lanthanum hexaboride layer, which seriously affects the corrosion resistance of the coating and introduces more impurities during the test.

[0065] Comparative Example 4

[0066] A method for preparing a nickel-based interface cone with a coating comprises the following steps:

[0067] (1) Pretreatment: Soak the interface cone in the cleaning solution for 10 minutes and dry it for 10 minutes;

[0068] (2) Pre-sputtering: Place the nickel-based interface cone into the magnetron sputtering chamber, evacuate the chamber, and introduce inert gas into the chamber to maintain the pressure in the chamber at 1×10 -1 Pa; close the sputtering baffle, and sputter nickel boride, titanium boride, zirconium boride, tantalum boride and lanthanum hexaboride targets one by one, with a sputtering power of 30 W and a sputtering time of 15 min;

[0069] (3) Sputtering coating: The nickel-based interface cone was heated to 250 °C and maintained for 5 min. The magnetron sputtering chamber was inert atmosphere and the pressure was maintained at 5 × 10-1 Pa; open the sputtering baffle, turn on the magnetron sputtering power supply of the nickel boride target, adjust the power to 40W, the sputtering time to 4min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the titanium boride target, adjust the power to 70W, the sputtering time to 3min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the zirconium boride target, adjust the power to 85W, the sputtering time to 4min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the tantalum boride target, adjust the power to 100W, the sputtering time to 4min, and turn off the magnetron sputtering power supply after completion; turn on the magnetron sputtering power supply of the lanthanum hexaboride target, adjust the power to 70W, the sputtering time to 5min, and turn off the magnetron sputtering power supply after completion;

[0070] (4) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 350℃ and keep it for 2h, then take out the interface cone after cooling for 6.5h.

[0071] The nickel-based interface cone with multi-layer boride coating can withstand the high-temperature plasma bombardment of 4000-8000K, can work continuously for ≥56h, has a service life of 12 months, can withstand acid-base environment corrosion of pH≤3 and pH≥9, and the corrosion products do not fall off. The corrosion product introduction during the test is ≤0.5ppm; the prepared coating thickness is 1.1μm, the density is ≥99.8%, the purity is ≥99.99%, the grain size is ≤1μm, the surface roughness is <0.5μm, and the thermal conductivity is ≥110W / m·K. This comparative example increases the sputtering time and sputtering power during the sputtering process, and significantly increases the coating thickness.

[0072] The invention provides a nickel-based interface cone coating, a nickel-based interface cone and a preparation method. A multilayer boride coating is prepared on the surface of the nickel-based interface cone by a vacuum magnetron sputtering process, wherein the innermost layer is a nickel boride coating, which can form a coating with a tight bond and high strength with the nickel-based interface cone, the middle coating is other metal boride coatings, which have high hardness, strength and thermal conductivity, and can provide support for the boride multilayer film, and the outermost layer is a lanthanum hexaboride coating, which has good chemical stability and reduces the introduction of other impurity atoms during the detection process. Compared with the platinum group metal coating, the coating saves 10%-20% of the preparation cost. The nickel-based interface cone coated with the coating can withstand the bombardment of high-temperature plasma of 4000-8000K, can work continuously for ≥56h, and has a service life of 12-24 months; the nickel-based interface cone coated with the coating can also withstand acid-base environment corrosion of pH≤3 and pH≥9, and the corrosion products do not fall off, and the introduction of corrosion products is ≤0.5ppm during detection.

[0073] Some exemplary embodiments of the present invention are described above. It can be understood that the above embodiments are only used to explain the present invention and do not constitute a limitation on the protection scope of the present invention. The features in these embodiments can be recombined in a suitable manner, and the scheme obtained thereby is still within the protection scope required by the present invention. Based on the above embodiments, all other embodiments obtained by those skilled in the art without making creative work, that is, all modifications, equivalent substitutions and improvements made within the spirit and principles of this application, fall within the protection scope required by the present invention.

Claims

1. A nickel-based interface cone coating, characterized in that: The coating is a multilayer boride coating, which includes a nickel boride layer, other metal boride layers and a lanthanum hexaboride layer, the nickel boride layer is the innermost layer, the lanthanum hexaboride layer is the outermost layer, and the other metal boride layers include one or more elements of tantalum, tungsten, zirconium, molybdenum, titanium and cerium.

2. A nickel-based interface cone coating according to claim 1, characterized in that: The coating has a thickness of 0.3-0.5 μm, and / or a density of ≥99.8%, and / or a purity of ≥99.99%, and / or a grain size of ≤1 μm, and / or a surface roughness of <0.5 μm.

3. A nickel-based interface cone coating according to claim 2, characterized in that: The thermal conductivity of the coating is ≥110 W / m·K, and / or the coating can withstand plasma bombardment of 4000-8000 K, and / or the coating can continuously work for ≥56 h, and / or the service life of the coating is 12-24 months, and / or the coating can withstand corrosion in an acid-base environment with a pH value of ≤3 and a pH value of ≥9, and the corrosion products do not fall off, and the corrosion products introduced during detection are ≤0.5 ppm.

4. A nickel-based interface cone with a coating as claimed in any one of claims 1 to 3.

5. A method for preparing a nickel-based interface cone with a coating as claimed in claim 4, characterized in that: The following steps are involved: (1) Pre-sputtering: The nickel-based interface cone is placed in the magnetron sputtering chamber. The magnetron sputtering chamber is inert atmosphere and the pressure is maintained at 1×10 -1 -3×10 -1 Pa; close the sputtering baffle, and sputter nickel boride, one or more other metal borides and lanthanum hexaboride targets one by one, with a sputtering power of 30-150W and a sputtering time of 3-15min; (2) Sputtering coating: Heat the nickel-based interface cone to 100-250°C and maintain for 5-15 min. The magnetron sputtering chamber is inert atmosphere and the pressure is maintained at 2×10 -1 -5×10 -1 Pa; open the sputtering baffle, and sputter the nickel boride coating, one or more other metal boride coatings and the lanthanum hexaboride coating in sequence, the sputtering power is 40-80W, the sputtering time of each coating layer is 2-8min, and the total sputtering time is ≤14min; (3) Coating heat treatment: After sputtering, the pressure in the magnetron sputtering chamber is maintained at 2×10 -4 Pa, heat the nickel-based interface cone to 200-500℃ and keep it for 0.5-3h, then cool it for 5-8h and take out the interface cone.

6. The method for preparing a nickel-based interface cone with a coating according to claim 5, characterized in that: Before pre-sputtering, the nickel-based interface cone is immersed in a mixed solution of hydrochloric acid: sulfuric acid with a volume ratio of 1:0.9-1.2 for 5-15 minutes and then dried for 10-30 minutes. The concentrations of the hydrochloric acid and the sulfuric acid are both ≤10%.

7. The method for preparing a nickel-based interface cone with a coating according to claim 5, characterized in that: The sputtering power supply is an AC power supply.

8. The method for preparing a nickel-based interface cone with a coating according to claim 5, characterized in that: The boride target material described in step (1) and step (2) is a boride of one element selected from the group consisting of nickel, lanthanum, tantalum, tungsten, zirconium, molybdenum, titanium and cerium. The purity of the boride target material is ≥99.99% and the grain size is ≤20 μm.

Images