Nickel-chromium alloy target material and preparation method thereof

Abstract

The invention provides a nickel-chromium alloy target material and a preparation method thereof, and belongs to the technical field of metal target materials. The preparation method of the nickel-chromium alloy target material comprises the following steps that a mold containing nickel-chromium mixed powder is subjected to hot pressing sintering treatment, a nickel-chromium alloy sintered body is obtained, machining is conducted, and the nickel-chromium alloy target material is obtained; wherein the hot pressing sintering treatment comprises three sections of heat preservation, the pressure of the first section of heat preservation is smaller than 1 MPa, the pressure of the second section of heat preservation is 6-10 MPa, and the pressure of the third section of heat preservation is 30-40 MPa. According to the hot pressing sintering treatment process, three-stage heat preservation is adopted, the pressure of each stage in the three-stage heat preservation process is controlled, the oxygen content and the grain size of the nickel-chromium alloy target material are reduced on the basis that the density of the target material is guaranteed, meanwhile, the grain orientation of the nickel-chromium alloy target material is controlled, and the quality of a sputtering film is effectively guaranteed.

Description

Technical Field

[0001] The present application relates to the technical field of metal target materials, and in particular to a nickel-chromium alloy target material and a preparation method thereof. Background Art

[0002] In the coating industry, the nickel-chromium alloy target prepared by adding Cr elements to high-purity Ni has excellent properties such as heat resistance, wear resistance, and corrosion resistance, making it widely used in high-end technology industries such as surface strengthening films, low-emissivity (Low-E) glass, microelectronics, magnetic recording, semiconductors, and thin film resistors. Therefore, the demand for nickel-chromium alloy targets is increasing, and the requirements for their performance, such as density, purity, grain size and distribution, uniformity, and grain orientation, are also higher. At present, nickel-chromium alloy targets are mainly prepared by powder metallurgy and smelting methods, but powder metallurgy and smelting methods can only control the grain size of nickel-chromium alloy targets to 40-50μm, and the grain orientation is random and the oxygen content is high.

[0003] In summary, there is an urgent need to develop a method for preparing a nickel-chromium alloy target, reduce the oxygen content and grain size of the nickel-chromium alloy target, and control the grain orientation of the nickel-chromium alloy target. Summary of the invention

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a nickel-chromium alloy target and a preparation method thereof.

[0005] To achieve the above object, the technical solution adopted by the present disclosure is: a method for preparing a nickel-chromium alloy target, comprising the following steps:

[0006] Hot pressing and sintering the mold filled with nickel-chromium mixed powder to obtain a nickel-chromium alloy sintered body, and machining the mold to obtain a nickel-chromium alloy target;

[0007] The hot pressing sintering process is a three-stage heat preservation process, wherein the heat preservation pressure of the first stage is less than 1MPa, the heat preservation pressure of the second stage is 6-10MPa, and the heat preservation pressure of the third stage is 30-40MPa.

[0008] In some embodiments, the hot pressing sintering process includes the following:

[0009] S1: Place the mold containing the nickel-chromium mixed powder into a hot pressing sintering furnace, evacuate to below 5Pa, heat to 800-1000℃ and keep warm for 30-60min, wherein the holding pressure is less than 1MPa;

[0010] S2: After the heat preservation in step S1 is completed, the temperature is raised to 1000-1100°C and the pressure is raised to 6-10MPa, and the temperature and pressure are maintained for 30-60 minutes;

[0011] S3: After the heat preservation in step S2 is completed, the temperature is increased to 1100-1200° C. and kept at this temperature for 30-60 minutes; after the heat preservation is completed, the pressure is increased to 30-40 MPa and kept at this temperature and pressure for 90-150 minutes.

[0012] In some embodiments, the heating step of step S1 is: placing the mold containing the nickel-chromium mixed powder into a hot pressing sintering furnace, evacuating to below 5 Pa, heating to 600-800°C at a heating rate of 8-10°C / min, and then heating to 800-1000°C at a heating rate of 5-8°C / min.

[0013] In some embodiments, the heating rate of step S2 is 4-5°C / min;

[0014] And / or, the heating rate of step S3 is 2-3°C / min;

[0015] And / or, the pressure increasing rate of step S3 is 0.25-0.35 MPa / min.

[0016] In some embodiments, before the hot pressing sintering process, a pre-pressing process is further included;

[0017] Preferably, the pre-pressing treatment step is: placing the mold filled with the nickel-chromium mixed powder into a hot pressing sintering furnace, increasing the pressure to 6-10 MPa at a pressure increasing rate of 0.1-0.3 MPa / min, and maintaining the pressure for 10-15 minutes.

[0018] In some embodiments, the nickel-chromium mixed powder is obtained by mixing nickel powder and chromium powder, and the mass of the chromium powder is 40-50% of the mass of the nickel-chromium mixed powder;

[0019] Preferably, the average particle size of the nickel powder is 8-10 μm;

[0020] Preferably, the average particle size of the chromium powder is 30-45 μm.

[0021] In some embodiments, the mixing is performed in a ball mill;

[0022] Preferably, the mixing is carried out by adding zirconium balls for dry mixing;

[0023] Preferably, the mass ratio of the zirconium balls to the materials is 1:1-3;

[0024] Preferably, the mixing is carried out under argon protection;

[0025] Preferably, the mixing time is 10-18h;

[0026] Preferably, the rotation speed of the ball mill is 300-400r / min.

[0027] In some embodiments, the mold is a graphite mold.

[0028] In some embodiments, the machining includes wire cutting and / or grinding; preferably, after the machining in step (3), the nickel-chromium alloy sputtering target is welded to a back plate, and then machined to a target size, followed by inspection, cleaning, drying and packaging to obtain a nickel-chromium alloy target assembly.

[0029] On the other hand, a nickel-chromium alloy target is provided, which is prepared using the method for preparing the nickel-chromium alloy target.

[0030] Compared with the prior art, the beneficial effects of the present invention are as follows: the hot pressing sintering process of the present application adopts three-stage heat preservation and controls the pressure at each stage of the three-stage heat preservation process. On the basis of ensuring the density of the target material, the oxygen content and grain size of the nickel-chromium alloy target material are reduced, and the grain orientation of the nickel-chromium alloy target material is controlled at the same time, thereby effectively ensuring the quality of the sputtered film. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 This is a metallographic morphology image of the sputtering surface of the nickel-chromium alloy target obtained in Example 1. DETAILED DESCRIPTION

[0032] In order to facilitate understanding of the present disclosure, the present disclosure will be described more fully below. However, the present disclosure can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present disclosure more thorough and comprehensive.

[0033] As used herein:

[0034] "Prepared from" is synonymous with "comprising." As used herein, the terms "comprising," "including," "having," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises the listed elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

[0035] The conjunction "consisting of excludes any unspecified element, step, or component. If used in a claim, this phrase renders the claim closed-ended so that it does not include materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of" appears in a clause of the body of a claim rather than immediately following the subject matter, it limits only the elements described in that clause; other elements are not excluded from the claim as a whole.

[0036] When amount, concentration or other value or parameter is represented by range, preferred range or a series of upper preferred value and lower preferred value, this should be understood as specifically disclosing all ranges formed by any pairing of any range upper limit or preferred value and any range lower limit or preferred value, regardless of whether the range is disclosed separately. For example, when disclosing range "1-5", described range should be interpreted as including range "1-4", "1-3", "1-2", "1-2 and 4-5", "1-3 and 5" etc. When numerical range is described in this article, unless otherwise stated, the range is intended to include its end value and all integers and fractions within the range.

[0037] In these examples, parts and percentages are by mass unless otherwise indicated.

[0038] "Parts by mass" refers to the basic unit of measurement for expressing the mass ratio of multiple components. 1 part can represent any unit mass, such as 1g or 2.689g. If we say that the mass of component A is a parts and the mass of component B is b parts, it means the ratio of the mass of component A to the mass of component B is a:b. Alternatively, it means that the mass of component A is aK and the mass of component B is bK (K is an arbitrary number, indicating a multiple factor). It should not be misunderstood that, unlike the mass parts, the sum of the mass of all components is not limited to 100 parts.

[0039] "And / or" is used to indicate that one or both of the stated situations may occur, for example, A and / or B includes (A and B) and (A or B).

[0040] In order to solve the problems of high oxygen content, large grain size and difficult to control grain orientation of nickel-chromium alloy targets in the prior art, the present disclosure provides a method for preparing a nickel-chromium alloy target, comprising the following steps:

[0041] Hot pressing and sintering the mold filled with nickel-chromium mixed powder to obtain a nickel-chromium alloy sintered body, and machining the mold to obtain a nickel-chromium alloy target;

[0042] The hot pressing sintering process is a three-stage heat preservation process, wherein the heat preservation pressure of the first stage is less than 1MPa, the heat preservation pressure of the second stage is 6-10MPa, and the heat preservation pressure of the third stage is 30-40MPa.

[0043] The hot pressing sintering process of the present application adopts three-stage heat preservation and controls the pressure in each stage of the three-stage heat preservation process. On the basis of ensuring the density of the target material, the oxygen content and grain size of the nickel-chromium alloy target material are reduced, and the grain orientation of the nickel-chromium alloy target material is controlled, thereby effectively ensuring the quality of the sputtered film.

[0044] Specifically, the temperature of the first insulation stage is 800-1000°C, the temperature of the second insulation stage is 1000-1100°C, and the temperature of the third insulation stage is 1100-1200°C.

[0045] Specifically, the temperature difference between the second insulation stage and the first insulation stage is greater than 100°C, and the temperature difference between the third insulation stage and the second insulation stage is greater than 50°C.

[0046] The present invention further reduces the oxygen content and grain size of the nickel-chromium alloy target material and improves the grain orientation of the nickel-chromium alloy target material by controlling the temperature during the three-stage insulation process and the temperature difference between each insulation stage.

[0047] In some embodiments, the hot pressing sintering process includes the following:

[0048] S1: Place the mold containing the nickel-chromium mixed powder into a hot pressing sintering furnace, evacuate to below 5Pa, heat to 800-1000℃ and keep warm for 30-60min, wherein the holding pressure is less than 1MPa;

[0049] S2: After the heat preservation in step S1 is completed, the temperature is raised to 1000-1100°C and the pressure is raised to 6-10MPa, and the temperature and pressure are maintained for 30-60 minutes;

[0050] S3: After the heat preservation in step S2 is completed, the temperature is increased to 1100-1200° C. and kept at this temperature for 30-60 minutes; after the heat preservation is completed, the pressure is increased to 30-40 MPa and kept at this temperature and pressure for 90-150 minutes.

[0051] The temperature in the hot pressing sintering step S1 of the present disclosure is raised to 800-1000°C, for example, but not limited to 800°C, 820°C, 840°C, 860°C, 880°C, 900°C, 920°C, 940°C, 960°C, 980°C, 1000°C;

[0052] The heat preservation for 30-60 minutes in the hot pressing sintering step S1 of the present disclosure may be, for example but not limited to, 30 minutes, 35 minutes, 40 minutes, 45 minutes, 50 minutes, 55 minutes, or 60 minutes;

[0053] The temperature in the hot pressing sintering step S2 of the present disclosure is raised to 1000-1100° C., for example, but not limited to 1000° C., 1020° C., 1040° C., 1060° C., 1080° C., 1100° C.;

[0054] The pressure increased to 6-10 MPa in the hot pressing sintering step S2 of the present disclosure may be, for example but not limited to, 6 MPa, 6.5 MPa, 7 MPa, 7.5 MPa, 8 MPa, 8.5 MPa, 9 MPa, 9.5 MPa, 10 MPa;

[0055] The heat preservation and pressure holding for 30-60 minutes in the hot pressing and sintering treatment step S2 of the present disclosure may be, for example, but not limited to, 30 minutes, 35 minutes, 40 minutes, 45 minutes, 50 minutes, 55 minutes, and 60 minutes;

[0056] The temperature in the hot pressing sintering step S2 of the present disclosure is raised to 1100-1200° C., for example, but not limited to 1100° C., 1120° C., 1140° C., 1160° C., 1180° C., 1200° C.;

[0057] The pressure increased to 30-40 MPa in the hot pressing sintering step S2 of the present disclosure may be, for example but not limited to, 30 MPa, 31 MPa, 32 MPa, 33 MPa, 34 MPa, 35 MPa, 36 MPa, 37 MPa, 38 MPa, 39 MPa, 40 MPa;

[0058] The heat preservation and pressure preservation for 90-150 minutes in the hot pressing and sintering treatment step S2 described in the present disclosure may be, for example, but not limited to, 90 minutes, 100 minutes, 110 minutes, 120 minutes, 130 minutes, 140 minutes, and 150 minutes.

[0059] Specifically, the temperature difference between the hot pressing and sintering step S2 and the hot pressing and sintering step S1 is greater than 100°C, preferably 150-250°C, for example, 100°C, 120°C, 150°C, 160°C, 180°C, 200°C, 220°C, 250°C;

[0060] Specifically, the temperature difference between the hot pressing and sintering step S3 and the hot pressing and sintering step S2 is greater than 50°C, preferably 70-100°C, for example, 70°C, 80°C, 90°C, 100°C;

[0061] In some embodiments, the heating step of step S1 is: placing the mold containing the nickel-chromium mixed powder into a hot pressing sintering furnace, evacuating to below 5 Pa, heating to 600-800°C at a heating rate of 8-10°C / min, and then heating to 800-1000°C at a heating rate of 5-8°C / min.

[0062] In the heating step of step S1, the temperature is firstly increased rapidly and then slowly increased, which is beneficial to remove oxygen in the nickel-chromium alloy target material and reduce the oxygen content of the nickel-chromium alloy target material.

[0063] In some embodiments, the heating rate of step S2 is 4-5°C / min; for example, it may be but is not limited to 4°C / min, 4.2°C / min, 4.4°C / min, 4.6°C / min, 4.8°C / min, 5°C / min;

[0064] In some embodiments, the heating rate of step S3 is 2-3°C / min; for example, it may be but is not limited to 2°C / min, 2.2°C / min, 2.4°C / min, 2.6°C / min, 2.8°C / min, 3°C / min;

[0065] In some embodiments, the pressure increase rate of step S3 is 0.1-0.3 MPa / min; for example, it may be but not limited to 0.1 MPa / min, 0.12 MPa / min, 0.15 MPa / min, 0.17 MPa / min, 0.2 MPa / min, 0.23 MPa / min, 0.25 MPa / min, 0.28 MPa / min, 0.3 MPa / min;

[0066] In some embodiments, the pressure increase rate of step S3 is 0.25-0.35 MPa / min; for example, it can be but not limited to 0.25 MPa / min, 0.28 MPa / min, 0.3 MPa / min, 0.32 MPa / min, 0.35 MPa / min.

[0067] In some embodiments, after the temperature in the hot pressing sintering furnace in step S3 drops to 200° C., the blank in the mold is taken out to obtain a nickel-chromium alloy sintered body.

[0068] In some embodiments, before the hot pressing sintering process, a pre-pressing process is further included;

[0069] Preferably, the pre-pressing treatment step is: placing the mold filled with the nickel-chromium mixed powder into a hot pressing sintering furnace, increasing the pressure to 6-10 MPa at a pressure increasing rate of 0.1-0.3 MPa / min, and maintaining the pressure for 10-15 minutes.

[0070] The present invention performs a pre-pressing treatment before the hot pressing sintering treatment, which can achieve the initial density requirement required for the hot pressing sintering treatment, thereby ensuring that after the subsequent hot pressing sintering treatment, a nickel-chromium alloy target with a density of >94% can be obtained.

[0071] In some embodiments, the nickel-chromium mixed powder is obtained by mixing nickel powder and chromium powder, and the mass of chromium powder is 40-50% of the mass of the nickel-chromium mixed powder; for example, it can be but not limited to 40%, 42%, 44%, 46%, 48%, 50%;

[0072] Preferably, the average particle size of the nickel powder is 8-10 μm;

[0073] Preferably, the average particle size of the chromium powder is 30-45 μm.

[0074] In some embodiments, the mixing is performed in a ball mill;

[0075] Preferably, the mixing is carried out by adding zirconium balls for dry mixing;

[0076] Preferably, the ball-to-material mass ratio of the zirconium ball is 1:1-3; for example, it can be but not limited to 1:1, 1:1.2, 1:1.5, 1:1.7, 1:2, 1:2.3, 1:2.5, 1:2.8, 1:3;

[0077] It is worth noting that the ball material mass ratio disclosed in the present invention refers to the ratio between the mass of the zirconium ball and the total mass of the nickel-chromium mixed powder.

[0078] Preferably, the mixing is carried out under argon protection;

[0079] Preferably, the mixing time is 10-18 hours; for example, it can be but not limited to 10 hours, 12 hours, 14 hours, 16 hours, 18 hours;

[0080] Preferably, the rotation speed of the ball mill is 300-400 r / min; for example, it can be but not limited to 300 r / min, 320 r / min, 340 r / min, 360 r / min, 380 r / min, 400 r / min.

[0081] Specifically, the preparation method of the nickel-chromium mixed powder is: add 50-60% by mass of nickel powder and 40-50% by mass of chromium powder into a polyurethane mixing barrel, then add zirconium balls according to a ball-to-material mass ratio of 1:1-3, fill the mixing barrel with argon gas, and after the filling is completed, ball mill the mixing barrel on a drum ball mill at a speed of 300-400r / min for 10-18h.

[0082] The nickel-chromium mixed powder prepared by the above method can not only ensure that the nickel powder and the chromium powder are mixed evenly, but also avoid the introduction of impurities, thereby improving the purity of the nickel-chromium alloy target material.

[0083] In some embodiments, the mold is a graphite mold.

[0084] In some embodiments, the machining includes wire cutting and / or grinding; preferably, after the machining in step (3), the nickel-chromium alloy sputtering target is welded to a back plate, and then machined to a target size, followed by inspection, cleaning, drying and packaging to obtain a nickel-chromium alloy target assembly.

[0085] On the other hand, a nickel-chromium alloy target is provided, which is prepared using the method for preparing the nickel-chromium alloy target.

[0086] The raw materials used in the embodiments and comparative examples are described below, but are not limited to these materials:

[0087] Nickel powder: commercially available, average particle size 10 μm, purity 99.95%;

[0088] Chromium powder: commercially available, average particle size 40 μm, purity 99.95%;

[0089] In the following examples and comparative examples,

[0090] The Ni-50wt% Cr mixed powder is homemade, and its preparation method is as follows: 50% by mass of nickel powder and 50% by mass of chromium powder are added into a polyurethane mixing powder barrel, and then zirconium balls are added according to the ball-to-material mass ratio of 1:2, and argon is continuously filled into the mixing powder barrel for 30 minutes. After the filling is completed, the mixing powder barrel is sealed, placed on a drum ball mill, and ball milled at a speed of 300r / min for 18 hours.

[0091] The Ni-40wt% Cr mixed powder is homemade, and its preparation method is as follows: add 60% by mass of nickel powder and 40% by mass of chromium powder into a polyurethane mixing powder barrel, and then add zirconium balls according to the ball-to-material mass ratio of 1:2, and continuously fill the mixing powder barrel with argon for 30 minutes. After the filling is completed, the mixing powder barrel is sealed, placed on a drum ball mill, and ball milled at a speed of 400r / min for 10 hours.

[0092] Example 1

[0093] This embodiment provides a method for preparing a nickel-chromium alloy target, comprising the following steps:

[0094] Pre-pressing treatment: Cut graphite paper of appropriate size to isolate the powder and graphite mold, put Ni-40wt%Cr mixed powder into the graphite mold, place it in a vacuum hot pressing sintering furnace, increase the pressure to 8MPa at a rate of 0.2MPa / min for pre-pressing, and release the pressure after maintaining the pressure for 10 minutes;

[0095] Hot pressing sintering treatment:

[0096] S1: Evacuate the pressure of the vacuum hot pressing sintering furnace to below 5Pa, start heating, first heat it to 600℃ at a heating rate of 10℃ / min, then heat it to 900℃ at a heating rate of 7℃ / min, and keep it warm for 45min, wherein the pressure of the hot pressing sintering furnace is controlled to be less than 1MPa;

[0097] S2: After the heat preservation in step S1 is completed, the temperature is increased to 1100°C at a heating rate of 5°C / min, the pressure is increased to 8MPa at a pressure increase rate of 0.2MPa / min, and the temperature and pressure are maintained for 45 minutes;

[0098] S3: After the heat preservation and pressure holding in step S2 is completed, the temperature is increased to 1200°C at a heating rate of 3°C / min and the temperature is kept for 45 minutes. After the heat preservation is completed, the pressure is increased to 40MPa at a pressure increase rate of 0.25MPa / min, and the temperature is kept for 120 minutes. After the heat preservation and pressure holding is completed, the hot pressing sintering furnace is closed and cooled. After the temperature in the hot pressing sintering furnace drops to 200°C, the blank in the mold is taken out to obtain a nickel-chromium alloy sintered body.

[0099] Machining: The nickel-chromium alloy sintered body obtained by hot pressing and sintering is machined to obtain a nickel-chromium alloy target.

[0100] Example 2

[0101] This embodiment provides a method for preparing a nickel-chromium alloy target, comprising the following steps:

[0102] Pre-pressing treatment: Cut graphite paper of appropriate size to isolate the powder and graphite mold, put Ni-40wt%Cr mixed powder into the graphite mold, place it in a vacuum hot pressing sintering furnace, increase the pressure to 8MPa at a rate of 0.2MPa / min for pre-pressing, and release the pressure after maintaining the pressure for 10 minutes;

[0103] Hot pressing sintering treatment:

[0104] S1: Evacuate the pressure of the vacuum hot pressing sintering furnace to below 5Pa, start heating, first heat it to 800℃ at a heating rate of 8℃ / min, then heat it to 1000℃ at a heating rate of 5℃ / min, and keep it warm for 60min, wherein the pressure of the hot pressing sintering furnace is controlled to be less than 1MPa;

[0105] S2: After the heat preservation in step S1 is completed, the temperature is increased to 1080°C at a heating rate of 4°C / min, the pressure is increased to 8MPa at a pressure increasing rate of 0.3MPa / min, and the temperature and pressure are maintained for 60 minutes;

[0106] S3: After the heat preservation and pressure holding in step S2 is completed, the temperature is increased to 1170°C at a heating rate of 3°C / min and the temperature is kept for 60 minutes. After the heat preservation is completed, the pressure is increased to 35MPa at a pressure increase rate of 0.35MPa / min, and the temperature is kept for 90 minutes. After the heat preservation and pressure holding is completed, the hot pressing sintering furnace is closed and cooled. After the temperature in the hot pressing sintering furnace drops to 200°C, the blank in the mold is taken out to obtain a nickel-chromium alloy sintered body.

[0107] Machining: The nickel-chromium alloy sintered body obtained by hot pressing and sintering is machined to obtain a nickel-chromium alloy target.

[0108] Example 3

[0109] This embodiment provides a method for preparing a nickel-chromium alloy target, comprising the following steps:

[0110] Pre-pressing treatment: Cut graphite paper of appropriate size to isolate the powder and graphite mold, put Ni-50wt%Cr mixed powder into the graphite mold, place it in a vacuum hot pressing sintering furnace, increase the pressure to 8MPa at a rate of 0.2MPa / min for pre-pressing, and release the pressure after maintaining the pressure for 10 minutes;

[0111] Hot pressing sintering treatment:

[0112] S1: Evacuate the pressure of the vacuum hot pressing sintering furnace to below 5Pa, start heating, first heat it to 600℃ at a heating rate of 10℃ / min, then heat it to 900℃ at a heating rate of 7℃ / min, and keep it warm for 30min, wherein the pressure of the hot pressing sintering furnace is controlled to be less than 1MPa;

[0113] S2: After the heat preservation in step S1 is completed, the temperature is increased to 1000°C at a heating rate of 5°C / min, the pressure is increased to 8MPa at a pressure increase rate of 0.2MPa / min, and the temperature and pressure are maintained for 30 minutes;

[0114] S3: After the heat preservation and pressure holding in step S2 is completed, the temperature is increased to 1120°C at a heating rate of 3°C / min and the temperature is kept for 30 minutes. After the heat preservation is completed, the pressure is increased to 30MPa at a pressure increase rate of 0.25MPa / min, and the temperature is kept for 150 minutes. After the heat preservation and pressure holding is completed, the hot pressing sintering furnace is closed and cooled. After the temperature in the hot pressing sintering furnace drops to 200°C, the blank in the mold is taken out to obtain a nickel-chromium alloy sintered body.

[0115] Machining: The nickel-chromium alloy sintered body obtained by hot pressing and sintering is machined to obtain a nickel-chromium alloy target.

[0116] Example 4

[0117] The present embodiment provides a method for preparing a nickel-chromium alloy target, which differs from the first embodiment only in that the step S2 in the hot pressing sintering process is different. The step S2 of the present embodiment is as follows: after the heat preservation of the first embodiment is completed, the temperature is increased to 1100°C at a heating rate of 5°C / min, the pressure is increased to 6MPa at a pressure increasing rate of 0.2MPa / min, and the temperature and pressure are maintained for 45 minutes; the remaining steps and parameters are the same as those of the first embodiment.

[0118] Example 5

[0119] The present embodiment provides a method for preparing a nickel-chromium alloy target, which differs from the first embodiment only in that the step S2 in the hot pressing sintering process is different. The step S2 of the present embodiment is as follows: after the heat preservation of the first embodiment is completed, the temperature is increased to 1100°C at a heating rate of 5°C / min, the pressure is increased to 10MPa at a pressure increasing rate of 0.2MPa / min, and the temperature and pressure are maintained for 45 minutes; the remaining steps and parameters are the same as those of the first embodiment.

[0120] Example 6

[0121] The present embodiment provides a method for preparing a nickel-chromium alloy target, which differs from the first embodiment only in that the step S2 in the hot pressing sintering process is different. The step S2 of the present embodiment is as follows: after the heat preservation of the first embodiment is completed, the temperature is increased to 1070°C at a heating rate of 5°C / min, the pressure is increased to 8MPa at a pressure increasing rate of 0.2MPa / min, and the temperature and pressure are maintained for 45 minutes; the remaining steps and parameters are the same as those of the first embodiment.

[0122] Example 7

[0123] The present embodiment provides a method for preparing a nickel-chromium alloy target, which differs from the first embodiment only in that the step S2 in the hot pressing sintering process is different. The step S2 of the present embodiment is as follows: after the heat preservation of the first embodiment is completed, the temperature is increased to 1040°C at a heating rate of 5°C / min, the pressure is increased to 8MPa at a pressure increasing rate of 0.2MPa / min, and the temperature and pressure are maintained for 45 minutes; the remaining steps and parameters are the same as those of the first embodiment.

[0124] Comparative Example 1

[0125] This comparative example provides a method for preparing a nickel-chromium alloy target, which differs from Example 1 only in that step S2 in the hot pressing sintering process is different. Step S2 of this comparative example is: after the insulation of step S1 is completed, the temperature is increased to 1100°C at a heating rate of 5°C / min, the pressure is increased to 4MPa at a pressure increase rate of 0.2MPa / min, and the temperature and pressure are maintained for 45 minutes; the remaining steps and parameters are the same as those in Example 1.

[0126] Comparative Example 2

[0127] This comparative example provides a method for preparing a nickel-chromium alloy target, which differs from Example 1 only in that step S2 in the hot pressing sintering process is different. Step S2 of this comparative example is: after the insulation of step S1 is completed, the temperature is increased to 1100°C at a heating rate of 5°C / min, the pressure is increased to 13MPa at a pressure increasing rate of 0.2MPa / min, and the temperature and pressure are maintained for 45 minutes; the remaining steps and parameters are the same as those in Example 1.

[0128] Comparative Example 3

[0129] This comparative example provides a method for preparing a nickel-chromium alloy target, which differs from Example 1 only in that step S2 in the hot pressing sintering process is different. Step S2 of this comparative example is: after the insulation of step S1 is completed, the temperature is increased to 1100°C at a heating rate of 5°C / min and kept warm for 45 minutes; the remaining steps and parameters are the same as those in Example 1.

[0130] Comparative Example 4

[0131] This comparative example provides a method for preparing a nickel-chromium alloy target, which differs from Example 1 only in that step S3 in the hot pressing and sintering treatment is different. Step S3 of this comparative example is: after the heat preservation and pressure holding in step S2 is completed, the temperature is increased to 1200°C at a heating rate of 3°C / min, the pressure is increased to 40MPa at a pressure increasing rate of 0.25MPa / min, and the heat preservation and pressure holding is performed for 120 minutes. After the heat preservation and pressure holding is completed, the hot pressing and sintering furnace is closed and cooled. After the temperature in the hot pressing and sintering furnace drops to 200°C, the blank in the mold is taken out to obtain a nickel-chromium alloy sintered body. The remaining steps and parameters are the same as those in Example 1.

[0132] The nickel-chromium alloy sputtering targets obtained in the above examples and comparative examples were subjected to the following performance tests:

[0133] (1) Density: tested by Archimedes drainage method;

[0134] (2) Density: The actual density of the nickel-chromium alloy sputtering target is measured according to the hanging basket method disclosed in the national standard GB / T 3850-2015 "Density measurement method for dense sintered metal materials and cemented carbide", and the theoretical density of the nickel-chromium alloy sputtering target is calculated according to the theoretical formula, which is calculated according to the calculation formula "density = actual density / theoretical density × 100%";

[0135] (3) Grain size: measured according to the cross-section method disclosed in the national standard GB / T 6394-2017 "Method for determination of average grain size of metals";

[0136] (4) Oxygen content: detected by oxygen, nitrogen and hydrogen detector;

[0137] (5) Cr content: detected by ICP equipment.

[0138] The test results are shown in Table 1 below.

[0139] Table 1

[0140]

[0141] It can be seen from the experimental data in Table 1 that the density of the nickel-chromium alloy target disclosed in the present invention is 7.91 g / cm 3The density is above 98.5%, the grain size is below 37μm, and the oxygen content is below 321ppm.

[0142] Figure 1 The metallographic morphology of the sputtering surface of the nickel-chromium alloy target obtained in Example 1 is shown in FIG. Figure 1 It can be seen that the nickel-chromium target has uniform microscopic distribution and small grain size, and it is easy to obtain a fine and uniform film during magnetron sputtering.

[0143] Finally, it should be noted that the above embodiments are used to illustrate the technical solution of the present disclosure rather than to limit the protection scope of the present disclosure. Although the present disclosure has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present disclosure can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present disclosure.

Claims

1. A method for preparing a nickel-chromium alloy target, characterized in that: The following steps are involved: Hot pressing and sintering the mold filled with nickel-chromium mixed powder to obtain a nickel-chromium alloy sintered body, and machining the mold to obtain a nickel-chromium alloy target; The hot pressing sintering process is a three-stage heat preservation process, wherein the heat preservation pressure of the first stage is less than 1MPa, the heat preservation pressure of the second stage is 6-10MPa, and the heat preservation pressure of the third stage is 30-40MPa.

2. The method for preparing a nickel-chromium alloy target according to claim 1, characterized in that: The hot pressing sintering process includes the following contents: S1: Place the mold containing the nickel-chromium mixed powder into a hot pressing sintering furnace, evacuate to below 5Pa, heat to 800-1000℃ and keep warm for 30-60min, wherein the holding pressure is less than 1MPa; S2: After the heat preservation in step S1 is completed, the temperature is raised to 1000-1100°C and the pressure is raised to 6-10MPa, and the temperature and pressure are maintained for 30-60 minutes; S3: After the heat preservation in step S2 is completed, the temperature is increased to 1100-1200° C. and kept at this temperature for 30-60 minutes; after the heat preservation is completed, the pressure is increased to 30-40 MPa and kept at this temperature and pressure for 90-150 minutes.

3. The method for preparing a nickel-chromium alloy target according to claim 2, characterized in that: The heating step of step S1 is as follows: placing the mold filled with nickel-chromium mixed powder into a hot pressing sintering furnace, evacuating to below 5 Pa, heating to 600-800°C at a heating rate of 8-10°C / min, and then heating to 800-1000°C at a heating rate of 5-8°C / min.

4. The method for preparing a nickel-chromium alloy target according to claim 2, characterized in that: The heating rate of step S2 is 4-5°C / min; And / or, the heating rate of step S3 is 2-3°C / min; And / or, the pressure increasing rate of step S3 is 0.25-0.35 MPa / min.

5. The method for preparing a nickel-chromium alloy target according to claim 1, characterized in that: Before the hot pressing and sintering process, a pre-pressing process is also included; Preferably, the pre-pressing treatment step is: placing the mold filled with the nickel-chromium mixed powder into a hot pressing sintering furnace, increasing the pressure to 6-10 MPa at a pressure increasing rate of 0.1-0.3 MPa / min, and maintaining the pressure for 10-15 minutes.

6. The method for preparing a nickel-chromium alloy target according to claim 1, characterized in that: The nickel-chromium mixed powder is obtained by mixing nickel powder and chromium powder, and the mass of the chromium powder is 40-50% of the mass of the nickel-chromium mixed powder; Preferably, the average particle size of the nickel powder is 8-10 μm; Preferably, the average particle size of the chromium powder is 30-45 μm.

7. The method for preparing a nickel-chromium alloy target according to claim 6, characterized in that: The mixing is carried out in a ball mill; Preferably, the mixing is carried out by adding zirconium balls for dry mixing; Preferably, the mass ratio of the zirconium balls to the materials is 1:1-3; Preferably, the mixing is carried out under argon protection; Preferably, the mixing time is 10-18h; Preferably, the rotation speed of the ball mill is 300-400r / min.

8. The method for preparing a nickel-chromium alloy target according to claim 1, characterized in that: The mold is a graphite mold.

9. The method for preparing a nickel-chromium alloy target according to claim 1, characterized in that: The machining includes wire cutting and / or grinding; preferably, after the machining in step (3), the nickel-chromium alloy sputtering target is welded to the back plate, and then machined to the target size, and then inspected, cleaned, dried and packaged in sequence to obtain a nickel-chromium alloy target assembly.

10. A nickel-chromium alloy target, characterized in that: The target is prepared by the method for preparing the nickel-chromium alloy target according to any one of claims 1 to 9.

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