CN115652269A - Manufacturing method of magnetic sputtering vacuum coating permanent magnet - Google Patents
Manufacturing method of magnetic sputtering vacuum coating permanent magnet Download PDFInfo
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Abstract
The invention discloses a method for manufacturing a magnetic sputtering vacuum coating permanent magnet, which belongs to the technical field of permanent magnet manufacturing and comprises the following steps: s1, preprocessing a base material, then placing a calibration material below and a base material above in a superposition sequence according to a certain distance sequence at a sputtering station, S2, mounting a target on a target base, then vacuumizing a coating chamber, and introducing protective gas. The ternary alloy film obtains finer grain size than the binary alloy film on the grain size, slows down the direct contact rate of corrosive liquid and matrix metal, greatly improves the corrosion resistance of the material, and in the actual production process, through utilizing the sintered Nd2Fe14B rare earth permanent magnet substandard product, is used for detecting the cleanliness of the target material, avoids losing the base material for detection, optimizes the processes of selective examination and full examination in the actual application process, and adopts a mass spectrometer for detection, so that the target material can be monitored, and the process is simple and efficient.
Description
Technical Field
The invention relates to the technical field of permanent magnet manufacturing, in particular to a manufacturing method of a magnetic sputtering vacuum coating permanent magnet.
Background
A magnet capable of maintaining its magnetism for a long period of time is called a permanent magnet. Such as natural magnets ((magnetite) and man-made magnets ((alnico), etc.) there are electromagnets that require power to be on for magnetic properties in addition to permanent magnets, which are also called hard magnets, are not easily demagnetized and are not easily magnetized, but their magnetic properties are reduced or eliminated if the permanent magnets are heated above the curie temperature or in an environment of high magnetic field strength in the opposite direction.
The magnetron sputtering method is to fill a proper amount of argon gas into high vacuum, apply a direct current voltage of several hundred K between a cathode (a columnar target or a planar target) and an anode (a coating chamber wall), and generate magnetic control type abnormal glow discharge in the coating chamber to ionize the argon gas.
The existing permanent magnet coating film is usually coated by adopting a magnetic sputtering instrument, the permanent magnet is usually coated with a corrosion-resistant film, in the actual production process, a large amount of base materials need to be extracted for detection, the compactness degree of the thickness of the coating film is determined, a large amount of waste is generated, in the magnetic sputtering process, a pre-sputtering flow exists, a large amount of electric power and consumables are wasted in the flow, in order to ensure the quality of the magnetic sputtering, a large amount of plasma is consumed, the raw materials are not fully utilized, in the subsequent selective inspection process, the cleanliness of the target materials can only be detected by the base sheets, and the detection flow is complicated.
Disclosure of Invention
The invention aims to provide a method for manufacturing a permanent magnet with a magnetic sputtering vacuum coating. According to the manufacturing method of the magnetic sputtering vacuum coating permanent magnet, disclosed by the invention, the nickel/aluminum/titanium ternary alloy film is lighter in cracking amplitude and less in falling after being subjected to neutral salt spray corrosion for 130h, the alloy film is better in storage integrity, continuity and uniformity, and better neutral salt spray corrosion resistance is obtained, the ternary alloy film obtains smaller grain size in grain size than the binary alloy film, grains are distributed in an island shape and are more dense, grain gaps are narrowed, corrosion channels among grains are correspondingly narrowed, so that the direct contact rate of a corrosion liquid and a matrix metal is slowed down, the corrosion resistance of a material is greatly improved, in the actual production process, the Nd2Fe14B rare earth permanent magnet inferior-quality product is sintered for detecting the cleanliness of the target, the loss of the base material is avoided, the processes of sampling inspection and full inspection are optimized in the actual application process, and the mass spectrometer is adopted for detection, so that the monitoring of the target can be realized, and the processes are simple and efficient.
In order to achieve the above effects, the present invention provides the following technical solutions: a manufacturing method of a magnetic sputtering vacuum coating permanent magnet is characterized by comprising the following steps:
s1, preprocessing a base material, and then placing a calibration material below and a base material above in a superposition sequence at a sputtering station according to a certain distance sequence.
S2, mounting the target on a target base, then carrying out vacuum pumping treatment in a coating chamber, and introducing protective gas.
And S3, moving the workpiece table to enable the calibration material to enter a magnetic sputtering station for waiting.
And S4, starting the magnetron sputtering instrument, performing direct current glow discharge, bombarding the material of the target, starting the magnetron mechanism, performing magnetron control on the substrate, restraining plasma, bombarding the target through the plasma, and adjusting through the workpiece table to enable the magnetic sputtering area to pre-sputter the calibration material.
And S5, moving the workpiece table, aligning the workpiece table to the base material for magnetic sputtering, completing bombardment on the target material according to the film coating sequence, performing full inspection on the calibration material of the same batch of base material by sampling, and performing quality detection.
Further, according to the operation step in S5,
s501, randomly sampling and inspecting a batch of base materials, cutting the base materials, and simultaneously taking down all the calibration materials.
S502, performing a corrosion test on the cut base material, stripping a calibration material coating, and then performing a mass spectrometer test to determine the coating mixing ratio.
S503, performing corrosion test, namely performing corrosion liquid by using low-concentration saline water, concentrated saline water and purified water, and assuming a control group.
And S504, cutting the edge of the base material, and performing microscopic examination by using a microscope to obtain the corrosion thickness of each coating.
And S505, finally, cleaning, drying and weighing the substrate, then stripping the rust layer by using a brush, and calculating the rust rate.
Further, according to the operation steps in S1, the base material is preferably a sintered Nd2Fe14B rare earth permanent magnet, the calibration material is a sintered Nd2Fe14B rare earth permanent magnet defective, the pretreatment is sanding, and then rough polishing is performed, the sample after rough polishing is sequentially heated and cleaned with acetone and alcohol in ultrasonic waves for 15min, and is continuously dried by blowing with ion wind after pretreatment, and is scrubbed with a thousand-grade cloth for standby.
Further, according to the operation step in S1, the target material is selected from an aluminum target material, a nickel target material and a titanium target material.
Further, according to the operation step in S2, the aluminum target and the titanium target are respectively mounted on two dc power source target bases, and the nickel target is mounted on the rf power source target base.
Further, according to the operation step in S4, the working air pressure of the target is kept at 1.0Pa, the temperature of the base material is normal temperature, the temperature is set to be 20-28 ℃, the rotating speed of the base material is 20 r.min < -1 >, the sputtering power of the target is 250W, and the uniform coating speed is about 0.3 nm.s < -1 >.
Further, according to the operation step in S2, the shielding gas is argon, and the pressure is set to 8 to 10pa.
Further, according to the operation step in S4, the thicknesses of the aluminum target, the nickel target, and the titanium target are 100 nm, 150 nm, and 200 nm, respectively.
Further, according to the operation step in S5, the shielding gas is argon gas, the argon gas pressure is 15 mtorr when standby, and the argon gas pressure is 10mtorr when the magnetic sputtering is turned on.
Further, according to the operation steps in S4, the pre-sputtering time is set to 10 minutes, the magnetic sputtering design is determined by the thickness of each plating layer, and the magnetron sputtering preparation process of the nickel/aluminum/titanium ternary alloy thin film is an argon gas flow value of 60sccm.
The invention provides a manufacturing method of a magnetic sputtering vacuum coating permanent magnet, which has the following beneficial effects: according to the manufacturing method of the magnetic sputtering vacuum coating permanent magnet, the nickel/aluminum/titanium ternary alloy film is lighter in cracking amplitude and less prone to falling off after being subjected to neutral salt spray corrosion for 130 hours, the alloy film is better in storage integrity, continuity and uniformity, and better neutral salt spray corrosion resistance is obtained, the ternary alloy film obtains smaller grain size in grain size than the binary alloy film, grains are distributed in island shape and are denser, grain gaps are narrowed, corrosion channels among grains are correspondingly narrowed, so that the direct contact rate of corrosive liquid and matrix metal is slowed down, the corrosion resistance of the material is greatly improved, in the actual production process, the sintered Nd2Fe14B rare earth permanent magnet defective products are used for detecting the cleanliness of the target, loss of the base material is avoided for detection, the processes of sampling inspection and full inspection are optimized in the actual application process, the target can be monitored by adopting a mass spectrometer for detection, and the process is simple and efficient.
Drawings
FIG. 1 is a schematic flow chart of a manufacturing method of a magnetic sputtering vacuum coating permanent magnet according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments below.
The invention provides a technical scheme that: referring to fig. 1, a method for manufacturing a magnetic sputtering vacuum coated permanent magnet includes the following steps:
s1, preprocessing a base material, and then placing a calibration material below and a base material above in a superposition sequence at a sputtering station according to a certain distance sequence.
S2, mounting the target on a target base, then carrying out vacuum pumping treatment in a coating chamber, and introducing protective gas.
And S3, moving the workpiece table to enable the calibration material to enter a magnetic sputtering station for waiting.
And S4, starting the magnetron sputtering instrument, performing direct current glow discharge, bombarding the material of the target, starting the magnetron mechanism, performing magnetron control on the substrate, restraining plasma, bombarding the target through the plasma, and adjusting through the workpiece table to enable the magnetic sputtering area to pre-sputter the calibration material.
And S5, moving the workpiece table, aligning the workpiece table to the base material for magnetic sputtering, completing bombardment on the target material according to the film coating sequence, performing full inspection on the calibration material of the same batch of base material by sampling, and performing quality detection.
Specifically, according to the operation procedure in S5,
s501, randomly sampling and inspecting a batch of base materials, cutting the base materials, and simultaneously taking down all the calibration materials.
S502, performing a corrosion test on the cut base material, stripping a calibration material coating, and then performing a mass spectrometer test to determine the coating mixing ratio.
S503, performing corrosion test, namely performing corrosion liquid by using low-concentration saline water, concentrated saline water and purified water, and assuming a control group.
And S504, cutting the edge of the base material, and performing microscopic examination by using a microscope to obtain the corrosion thickness of each coating.
And S505, finally, cleaning, drying and weighing the substrate, then stripping the rust layer by using a brush, and calculating the rust rate.
Specifically, according to the operation steps in S1, the base material is preferably a sintered Nd2Fe14B rare earth permanent magnet, the calibration material is a sintered Nd2Fe14B rare earth permanent magnet defective, the pretreatment is sanding with sand paper, and then rough polishing is performed, the sample after rough polishing is heated and cleaned with acetone and alcohol in ultrasonic waves for 15min, and then dried by continuous ion wind blowing after pretreatment, and scrubbed with thousand-grade cloth for standby.
Specifically, according to the operation step in S1, the target material is selected from an aluminum target material, a nickel target material, and a titanium target material.
Specifically, according to the operation steps in S2, the aluminum target and the titanium target are respectively mounted on two dc power source target bases, and the nickel target is mounted on the rf power source target base.
Specifically, according to the operation step in S4, the working air pressure of the target material is kept at 1.0Pa, the temperature of the base material is normal temperature, the temperature is set to be 20-28 ℃, the rotating speed of the base material is 20 r.min < -1 >, the sputtering power of the target material is 250W, and the uniform coating speed is about 0.3 nm.s < -1 >.
Specifically, according to the operation procedure in S2, the shielding gas is argon gas, and the pressure is set to 8-10Pa.
Specifically, according to the operation step in S4, the thicknesses of the aluminum target, the nickel target, and the titanium target are 100 nm, 150 nm, and 200 nm, respectively.
Specifically, according to the operation procedure in S5, the shielding gas is argon, the argon gas pressure is 15mto when standby, and the argon gas pressure is 10mtorr when the magnetic sputtering is started.
Specifically, according to the operation steps in S4, the pre-sputtering time is set to 10 minutes, the magnetic sputtering design is determined by the thickness of each plating layer, and the magnetron sputtering preparation process of the nickel/aluminum/titanium ternary alloy thin film is an argon gas flow value of 60sccm.
The purity test methods of the examples were performed for assay and compared to the prior art to obtain the following data:
| anti-rust performance | Convenience of operation | Convenience of detection | |
| Examples | Is higher than | Is higher than | Is higher than |
| Prior Art | In general | In general | In general |
According to the table data, in the embodiment, by the manufacturing method of the magnetic sputtering vacuum coating permanent magnet, after the nickel/aluminum/titanium ternary alloy film is subjected to neutral salt spray corrosion for 130 hours, the film is light in cracking amplitude, less in falling, better in preservation integrity, continuity and uniformity of the alloy film, and better in neutral salt spray corrosion resistance, the ternary alloy film obtains smaller grain size than the binary alloy film in grain size, the grains are distributed in an island shape and are more dense, grain gaps are narrowed, and corrosion channels among the grains are correspondingly narrowed, so that the direct contact rate of corrosive liquid and matrix metal is reduced, the corrosion resistance of the material is greatly improved, in the actual production process, the cleanliness of the Nd2Fe14B rare earth permanent magnet is detected by using a sintering inferior product, so that the loss of the base material is avoided, the processes of sampling inspection and full inspection are optimized in the actual application process, the mass spectrometer is adopted for detection, and the monitoring of the Nd2Fe14B rare earth permanent magnet can be realized, and the target material is simple and efficient.
The invention provides a method for manufacturing a magnetic sputtering vacuum coating permanent magnet, which is characterized by comprising the following steps of: s1, pretreating a base material, then placing the base material at a sputtering station according to a superposition sequence of a calibration material below and a base material above according to a certain distance sequence, wherein the base material is preferably sintered Nd2Fe14B rare earth permanent magnet, the calibration material is sintered Nd2Fe14B rare earth permanent magnet inferior product, the calibration material is pretreated into sand paper for polishing, then rough polishing is carried out, a sample after the rough polishing treatment is heated and cleaned for 15min in ultrasonic wave by acetone and alcohol, continuous ion wind blowing drying is carried out after the pretreatment, thousand-grade cloth is adopted for scrubbing for standby use, the target material is selected from aluminum target material, nickel target material and titanium target material, S2, the target material is installed on a target material base, then a coating chamber is vacuumized, protective gas is introduced, the aluminum target material and the titanium target material are respectively installed on two DC power supply target material bases, the nickel target material is installed on a radio frequency power supply target material base, the protective gas is argon, setting the pressure to be 8-10pa, S3, moving a workpiece table to enable a calibration material to enter a magnetic sputtering station for waiting, S4, starting a magnetron sputtering instrument, performing direct current glow discharge, bombarding a material of a target material, starting a magnetron mechanism, performing magnetron on a substrate, restraining plasma, bombarding the target material through the plasma, adjusting the workpiece table to enable a magnetic sputtering area to perform pre-sputtering on the calibration material, keeping the working pressure of the target material at 1.0Pa, setting the temperature of the substrate at normal temperature at 20-28 ℃, setting the rotating speed of the substrate at 20 r.min < -1 >, setting the sputtering power of the target material at 250W, setting the uniform coating speed at about 0.3 nm.s < -1 >, setting the thicknesses of an aluminum target material, a nickel target material and a titanium target material at 100 nm, 150 nm and 200 nm respectively, setting the pre-sputtering time at 10 minutes, setting the magnetic sputtering design to be determined by the thicknesses of various coating layers, and setting the magnetron sputtering preparation process of the nickel/aluminum/titanium ternary alloy film to be an argon flow value of 60sc cm, s5, moving a workpiece table, aligning a substrate to carry out magnetic sputtering, completing bombardment on a target according to a coating sequence, carrying out overall inspection on the same batch of substrates by sampling and inspecting a calibration material, carrying out quality detection, S501, randomly sampling and inspecting a batch of substrates, cutting the substrates, simultaneously taking down all the calibration material, S502, carrying out corrosion test on the cut substrates, stripping a coating of the calibration material, carrying out mass spectrometer test, determining a coating mixing ratio, S503, carrying out corrosion test, carrying out corrosive liquid by adopting low-concentration saline water, strong brine and purified water, assuming a comparison group, S504, carrying out edge cutting on the substrates, carrying out microscopic examination by adopting a microscope to obtain the corrosion thickness of each coating, S505, finally cleaning, drying and weighing the substrates, then stripping off a corrosion layer by using a brush, calculating the corrosion rate, taking argon as protective gas, and keeping the argon gas pressure at 15mtor in standby, argon pressure is 10mtorr when magnetic sputtering is started, a neutral salt spray corrosion test is carried out in an intelligent touch screen salt spray tester, a neutral salt spray solution used in the test is a NaCl solution with the mass fraction of 3.5% and a NaCl solution with the mass fraction of 7%, the pH value of salt spray is kept between 6.2 and 7.5, the temperature of a case of the intelligent touch screen salt spray tester is controlled to be (35 +/-2) ° C, the temperature of a saturated air barrel is kept to be (47 +/-1) ° C, the humidity is kept to be more than 95%, 1-2 mL/(h.cm & lt 2 & gt) is taken as a standard mist reduction amount, the pressure of a nozzle is adjusted to be 78.5-137.3 kPa (0.8-1.4 kgf/cm & lt 2 & gt), spraying is continuously carried out every day, salt spray is uniformly deposited on the surface of a sample, in the test, a digital camera is used for carrying out macroscopic recording on the sample every 20, 30, 50, 70, 90, 110 and 130h of pure water used in the neutral salt spray corrosion test is taken, the neutral salt spray corrosion test is modified into pure water under the same condition, as a comparison, the same batch of substrates are subjected to a secondary comparison at 35 ± 2 ℃ and a humidity lower than 5%, samples corroded by neutral salt fog are repeatedly washed in flowing clear water, slowly and lightly brushed by a fine soft brush, and then dehydrated in absolute ethyl alcohol, the samples are weighed after being dried, but no matter which cleaning method is adopted to remove corrosion products, the base metal is damaged to a certain extent, so that a certain error exists in the measured corrosion rate, one or more samples which are cleaned and weighed can be cleaned and weighed again by the same method in order to correct the artificially-caused error, and the corrected mass loss value is calculated according to formula (1), wherein VW = (W1-W2) - (W2-W3), wherein: Δ W is the corrected mass loss value; w1 is the sample quality before the corrosion test; w2 is the sample mass after the corrosion products are removed; w3 is the sample mass after the second washing,
the corrected corrosion rate is calculated according to equation (2):
in the formula: r is the corrected corrosion rate; k is a constant; s is the surface area of the sample; t is corrosion test time; d is the density, compared with an aluminum/nickel binary alloy film, the nickel/aluminum/titanium ternary alloy film has the advantages that the cracking amplitude of the film is smaller after the neutral salt spray corrosion for 130 hours, the falling is less, the storage integrity, the continuity and the uniformity of the alloy film are better, and the more excellent neutral salt spray corrosion resistance is obtained. The introduction of titanium may lead to a finer grain size of the ternary alloy film than that of the binary alloy film, the grains are arranged in an island shape and are denser, the grain gaps are narrowed, and the inter-grain corrosion channels are correspondingly narrowed, thereby slowing down the direct contact rate of the corrosive liquid and the matrix metal and greatly improving the corrosion resistance of the material.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A manufacturing method of a magnetic sputtering vacuum coating permanent magnet is characterized by comprising the following steps:
s1, preprocessing a base material, and then placing a calibration material below and a base material above in a superposition sequence at a sputtering station according to a certain distance sequence;
s2, mounting the target on a target base, then carrying out vacuum pumping treatment in a coating chamber, and introducing protective gas;
s3, moving the workpiece table to enable the calibration material to enter a magnetic sputtering station to wait;
s4, starting a magnetron sputtering instrument, performing direct current glow discharge to bombard the material of the target, starting a magnetron mechanism to perform magnetron control on the base material, restraining plasma, bombarding the target through the plasma, and adjusting through a workpiece table to enable a magnetic sputtering area to perform pre-sputtering on the calibration material;
and S5, moving the workpiece table, aligning the workpiece table to the base material for magnetic sputtering, completing bombardment on the target material according to the film coating sequence, performing full inspection on the calibration material of the same batch of base material by sampling, and performing quality detection.
2. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation procedure in S5,
s501, randomly sampling and inspecting a batch of base materials, cutting the base materials, and taking down all calibration materials;
s502, performing corrosion test on the cut base material, stripping a calibration material coating, and then performing mass spectrometer test to determine the coating mixing proportion;
s503, performing corrosion test, namely performing corrosion liquid by using low-concentration saline water, strong brine and purified water, and assuming a control group;
s504, cutting the edge of the base material, and performing microscopic examination by using a microscope to obtain the corrosion thickness of each coating;
and S505, finally, cleaning, drying and weighing the substrate, then stripping the rust layer by using a brush, and calculating the rust rate.
3. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation steps in the S1, the base material is preferably a sintered Nd2Fe14B rare earth permanent magnet, the calibration material is a sintered Nd2Fe14B rare earth permanent magnet defective product, the pretreatment is to polish with sand paper and then to perform rough polishing, the sample after the rough polishing is heated and cleaned with acetone and alcohol in ultrasonic waves for 15min, and then is dried by continuous ion wind blowing after the pretreatment, and is scrubbed with thousand-grade cloth for standby.
4. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation step in S1, the target material is selected from an aluminum target material, a nickel target material and a titanium target material.
5. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation steps in the S2, the aluminum target and the titanium target are respectively arranged on two direct current power supply target bases, and the nickel target is arranged on a radio frequency power supply target base.
6. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation step in S4, the working air pressure of the target material is kept at 1.0Pa, the temperature of the base material is normal temperature, the temperature is set to be 20-28 ℃, the rotating speed of the base material is 20 r.min < -1 >, the sputtering power of the target material is 250W, and the uniform coating speed is about 0.3 nm.s < -1 >.
7. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation step in S2, the protective gas is argon, and the pressure is set to be 8-10pa.
8. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation step in S4, the thicknesses of the aluminum target, the nickel target, and the titanium target are 100 nm, 150 nm, and 200 nm, respectively.
9. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation steps in S5, the protective gas is argon, the argon pressure is 15mto when the protective gas is standby, and the argon pressure is 10mtorr when the magnetic sputtering is started.
10. A method of manufacturing a magnetron sputtering vacuum coated permanent magnet as claimed in claim 1, comprising the steps of: according to the operation steps in S4, the pre-sputtering time is set to be 10 minutes, the magnetic sputtering design is determined by the thickness of each plating layer, and the magnetron sputtering preparation process of the nickel/aluminum/titanium ternary alloy film is that the argon gas flow value is 60sccm.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1456704A (en) * | 2002-05-10 | 2003-11-19 | 西门子公司 | Method for on-the-spot determining membrane thickness |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456704A (en) * | 2002-05-10 | 2003-11-19 | 西门子公司 | Method for on-the-spot determining membrane thickness |
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| Title |
|---|
| 杨英奇 等: "磁控溅射表面镀膜对Nd2Fe14B稀土永磁体抗腐蚀性能的影响" * |
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