CN112481666A - Samarium-iron-cobalt-phosphorus amorphous film and preparation method thereof - Google Patents
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Abstract
The invention discloses a samarium-iron-cobalt-phosphorus amorphous film, which comprises Sm, Fe, Co and P, wherein the weight percentage ratio of each element is Sm: fe: co: p ═ x: y: z: a, x is more than or equal to 5.0 and less than or equal to 35.0, y is more than or equal to 55.0 and less than or equal to 80.0, z is more than or equal to 0 and less than or equal to 30.0, a is more than or equal to 0.1 and less than or equal to 2.0, and x + y + z + a is equal to 100. The invention also discloses a preparation method of the samarium-iron-cobalt-phosphorus amorphous film, which comprises the following steps: (1) activating the electrode plate; (2) electrochemical codeposition; (3) and (5) cleaning the film. The method can realize the controllable codeposition of three elements of Sm, Fe and Co, the elements of the film are uniformly distributed, and the saturation magnetization intensity of the amorphous film prepared by the preparation method is higher and reaches 137 emu/g.
Description
Technical Field
The invention relates to the technical field of alloy and magnetic materials, in particular to a samarium-iron-cobalt-phosphorus amorphous film and a preparation method thereof.
Background
With the rapid development in the fields of rail transit, medical instruments, industrial motors and the like, the magnetic performance of permanent magnetic materials is required to be very high. At present, the magnetic property record of the permanent magnetic material is still kept by the neodymium iron boron series rare earth permanent magnetic material. Rare earth transition group nitrides, soft and hard magnetic nano composite magnets and the like have respective fatal scientific and technical problems.
The Sm (FeCo)12 type permanent magnetic alloy originates from SmFe12 type alloy, and is considered to be one of the most potential fourth-generation permanent magnetic materials because the Fe content is high, and the added Co element can generate a super exchange effect with the Fe element, thereby greatly improving the saturation magnetization, the magnetocrystalline anisotropy field and the Curie temperature. However, researches show that the traditional preparation processes such as induction melting, isothermal aging, melt rapid quenching, annealing, rapid hardening, casting and the like cannot obtain a single product 1: the 12-type alloy phase inevitably contains α -Fe in the magnet, and the addition of elements such as Ti/Zr can suppress the precipitation of α -Fe, but the saturation magnetic moment of the magnet is lowered by the magnetic dilution effect.
The amorphous crystal is widely applied to the preparation of difficult-to-extract alloy, but the alloy amorphous formed by rare earth element Sm and transition metal has weaker forming capability, and the preparation difficulty of an amorphous SmFeCo matrix is higher.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the invention provides a samarium-iron-cobalt-phosphorus amorphous film and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
a samarium iron cobalt phosphorus amorphous film comprises Sm, Fe, Co and P, wherein the weight percentage ratio of each element is Sm: fe: co: p ═ x: y: z: a, x is more than or equal to 5.0 and less than or equal to 35.0, y is more than or equal to 55.0 and less than or equal to 80.0, z is more than or equal to 0 and less than or equal to 30.0, a is more than or equal to 0.1 and less than or equal to 2.0, and x + y + z + a is equal to 100.
A preparation method of a samarium iron cobalt phosphorus amorphous film can be used for preparing the samarium iron cobalt phosphorus amorphous film, and comprises the following steps:
(1) activating an electrode slice:
the positive electrode is a platinum electrode plate, the platinum electrode plate is soaked in a mixed solution of acetone and ethanol for 5-15 min, and then the platinum electrode plate is dried;
the cathode material is tungsten or tantalum slice, soaking for 1-3 min by adopting a mixed solution of acetone and hydrochloric acid, and then drying;
(2) electrochemical co-deposition:
heating the electroplating solution to 40-80 ℃, wherein the pH value is 3.2-5.1, the distance between the anode and the cathode is 2-5 cm, and the current density is 0.5-1.2A/dm2The codeposition time is 10-45 min;
(3) cleaning a film:
ultrasonic wave and ethanol cleaning are adopted to obtain the samarium-iron-cobalt-phosphorus amorphous film.
Further, in the step (1), the volume fraction of acetone in the mixed solution of acetone and ethanol is 75-95%; in the mixed solution of acetone and hydrochloric acid, the volume fraction of acetone is 90-98%.
Further, in the step (1), the drying is carried out in Ar atmosphere at the temperature of 50-100 ℃ for 5-12 min.
Further, in the step (2): the plating solution comprises, by mass: 5-30g/L of phosphoric acid, 10-20 g/L of boric acid, 2-18 g/L of complexing agent, 3-8 g/L of additive, 10-25 g/L of iron salt, 12-40 g/L of samarium salt and 3-11 g/L of cobalt salt.
Further, the complexing agent is: at least one of aminocycloacid, glycine, arginine, ethylene glycol, benzene ring acid, citric acid and tartaric acid. The addition of the complexing agent is beneficial to the codeposition of Sm and Fe, and if no other complexing agent or other complexing agents are added, the deposition of Sm cannot be realized.
Further, the ferric salt is at least one of ferric chloride, ferrous sulfate, ferric nitrate, ferrous chloride tetrahydrate and ferrous nitrate.
Further, the cobalt salt is one or two of cobalt chloride and cobalt nitrate.
Further, the samarium salt is at least one of samarium chloride hexahydrate, anhydrous samarium chloride and samarium nitrate.
Further, the additive is at least one of sodium chloride, potassium chloride, sodium hypochlorite and sodium hypophosphite. The additive is mainly used as ion balance buffer in the reaction process and is also beneficial to the codeposition of Sm \ Fe \ Co to a certain extent.
Further, in the step (3), the purity of the ethanol is more than 99%, and the ultrasonic cleaning time is 2-6 min.
The invention has the beneficial effects that:
(1) the invention can realize the controllable codeposition of three elements of Sm, Fe and Co, and the elements of the film are uniformly distributed, thereby providing a new technology for preparing novel magnetic materials.
(2) The preparation method can realize the codeposition of the Sm-Fe-Co ternary alloy system, obtain the SmFeCo amorphous matrix with uniform component distribution and controllable element content, provide an excellent precursor for subsequent crystallization and other treatments, and ensure that the amorphous film has uniform element distribution and controllable element content.
(3) The Sm, Fe and Co elements in the amorphous film prepared by the method are uniformly distributed and do not present lamellar distribution. The oxygen content in the film prepared by the method is less than 500 ppm. The oxygen content is mainly derived from the plating solution, and as the oxygen content is lower, the better, the oxygen content is too high, which results in too much consumption of the element Sm of the thin film, difficulty in forming a magnetic phase, and deterioration of magnetic properties.
(4) Compared with the traditional method, the preparation method disclosed by the invention realizes one-time codeposition of the ternary alloy of Sm, Fe and Co, which cannot be realized in the traditional method, and the saturation magnetization intensity of the amorphous film prepared by the preparation method disclosed by the invention is higher and reaches 137 emu/g.
Drawings
FIG. 1 is a graph showing the results of surface morphology and element distribution of the amorphous thin film obtained in example 1, wherein (a) is the results of measurement of surface waviness of the amorphous thin film, and (b), (c), and (d) are elemental scans of Sm, Fe, and Co, respectively.
FIG. 2 shows X-ray diffraction results of the amorphous thin film prepared in example 1, which were measured by X-ray diffraction.
Fig. 3 is a demagnetization graph of the amorphous thin films prepared in example 1 and comparative example 1.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, and it should be noted that the detailed description is only for describing the present invention, and should not be construed as limiting the present invention.
Example 1
A preparation method of a samarium-iron-cobalt-phosphorus amorphous film comprises the following steps:
(1) activating an electrode slice:
the positive electrode is a platinum electrode plate, the platinum electrode plate is soaked by adopting a mixed solution of acetone and ethanol, the volume fraction of the mixed solution of acetone and ethanol is 75% in terms of volume ratio, the soaking time is 5min, and then the platinum electrode plate is dried.
The cathode material is a tungsten sheet with the purity not lower than 99.9 percent, and the tungsten sheet is soaked by mixed solution of acetone and hydrochloric acid, wherein the volume fraction of the acetone in the mixed solution of acetone and hydrochloric acid is 90 percent, the soaking time is 1min, and then the tungsten sheet is dried.
The drying process is carried out under Ar atmosphere, the temperature is 60 ℃, and the drying time is 5 min.
(2) Preparing the samarium iron cobalt phosphorus amorphous film by electrochemical codeposition:
heating the electroplating solution to 40 deg.C, pH 3.2, distance between positive and negative electrodes 2.5cm, and current density 0.5A/dm2And the codeposition time is 15min, and the samarium-iron-cobalt-phosphorus amorphous film is obtained.
Wherein the electroplating solution comprises the following components in percentage by mass: 5g/L phosphoric acid, 15g/L boric acid, 4g/L complexing agent, 3g/L additive, 25g/L iron salt, 12g/L samarium salt and 5g/L cobalt salt; the total mass concentration of the complexing agent is 4g/L, and the complexing agent is as follows: amino cyclic acid and glycine, wherein the mass concentration ratio of the amino cyclic acid to the glycine is 1: 1, the ferric salt is ferric chloride; the cobalt salt is cobalt chloride; the samarium salt is samarium chloride hexahydrate, and the additive is sodium chloride.
(3) Cleaning a film:
and cleaning the samarium-iron-cobalt-phosphorus amorphous film by adopting ultrasonic waves and ethanol, wherein the ultrasonic cleaning time is 3 min.
In this embodiment, the samarium-iron-cobalt-phosphorus amorphous thin film prepared by the method contains Sm, Fe, Co and P, wherein the weight ratio of each element is Sm: fe: co: p ═ 7: 66: 26.7: 0.3, the film thickness is 20 μm.
Example 2
A preparation method of a samarium-iron-cobalt-phosphorus amorphous film comprises the following steps:
(1) activating an electrode slice:
the positive electrode is a platinum electrode plate, the platinum electrode plate is soaked in a mixed solution of acetone and ethanol, the volume fraction of the acetone in the mixed solution of acetone and ethanol is 80% in volume ratio, the soaking time is 5min, and then the platinum electrode plate is dried.
The cathode material is a tungsten sheet with the purity of not less than 99.9 percent, and the tungsten sheet is soaked by mixed solution of acetone and hydrochloric acid, wherein the volume fraction of the acetone in the mixed solution of acetone and hydrochloric acid is 80 percent, the soaking time is 1min, and then the tungsten sheet is dried.
The drying process is carried out under Ar atmosphere at 60 deg.C for 5 min.
(2) Preparing the samarium iron cobalt phosphorus amorphous film by electrochemical codeposition:
heating the electroplating solution to 40 deg.C, pH 3.5, distance between positive and negative electrodes 2.5cm, and current density 0.8A/dm2And the codeposition time is 10min, and the samarium-iron-cobalt-phosphorus amorphous film is obtained.
Wherein the electroplating solution comprises the following components in percentage by mass: 10g/L of phosphoric acid, 12g/L of boric acid, 5g/L of complexing agent, 3g/L of additive, 20g/L of iron salt, 12g/L of samarium salt and 8g/L of cobalt salt; the complexing agent is: the complexing agent is 5g/L in total mass concentration, and the mass concentration ratio of the aminocyclic acid to the glycine to the citric acid is 2: 2: 1, the ferric salt is ferric chloride and ferrous chloride, the total mass concentration of the ferric salt is 20g/L, and the mass concentration ratio of the ferric chloride to the ferrous chloride is 1: 2; the cobalt salt is cobalt chloride; the samarium salt is anhydrous samarium chloride, the additive is sodium chloride and potassium chloride, and the mass concentration ratio of the sodium chloride to the potassium chloride is 1: 1.
(3) cleaning a film:
and cleaning the samarium-iron-cobalt-phosphorus amorphous film by adopting ultrasonic waves and ethanol, wherein the ultrasonic cleaning time is 3 min.
In this embodiment, the prepared samarium-iron-cobalt-phosphorus amorphous thin film contains Sm, Fe, Co and P, wherein the weight ratio of each element is Sm: fe: co: p is 10: 64: 25: 1, the film thickness is 20 μm.
Example 3
A preparation method of a samarium-iron-cobalt-phosphorus amorphous film comprises the following steps:
(1) activating an electrode slice:
the positive electrode is a platinum electrode plate, the platinum electrode plate is soaked by adopting a mixed solution of acetone and ethanol, the volume fraction of the mixed solution of acetone and ethanol is 75% in terms of volume ratio, the soaking time is 5min, and then the platinum electrode plate is dried.
The cathode material is a tungsten sheet with the purity of not less than 99.9 percent, and the tungsten sheet is soaked by mixed solution of acetone and hydrochloric acid, wherein in the mixed solution of acetone and hydrochloric acid, the volume fraction of acetone is 80 percent by volume, the soaking time is 1min, and then the tungsten sheet is dried.
The drying process is carried out under Ar atmosphere at 60 deg.C for 5 min.
(2) Preparing the samarium iron cobalt phosphorus amorphous film by electrochemical codeposition:
heating the electroplating solution to 40 deg.C, pH 4.0, distance between positive and negative electrodes 2.5cm, and current density 4.1A/dm2And the codeposition time is 30min, and the samarium-iron-cobalt-phosphorus amorphous film is obtained.
Wherein the electroplating solution comprises the following components in percentage by mass: 20g/L of phosphoric acid, 15g/L of boric acid, 12g/L of complexing agent, 8g/L of additive, 15g/L of iron salt, 30g/L of samarium salt and 7.5g/L of cobalt salt; the complexing agent is: amino cyclic acid, glycine and citric acid, wherein the total mass concentration of the complexing agent is 12g/L, and the mass concentration ratio of the amino cyclic acid to the glycine to the citric acid is 3: 3: 1, the ferric salt is ferric chloride and ferrous sulfate, the total mass concentration of the ferric salt is 15g/L, and the mass concentration of the ferric chloride and the ferrous sulfate is 1: 2; the cobalt salt is cobalt chloride; the samarium salt is samarium chloride hexahydrate, the additives are sodium chloride and potassium chloride, the total mass concentration of the additives is 8g/L, and the mass concentration ratio of the sodium chloride to the potassium chloride is 1: 1.
(3) cleaning a film:
and cleaning the samarium-iron-cobalt-phosphorus amorphous film by adopting ultrasonic waves and ethanol, wherein the ultrasonic cleaning time is 3 min.
In this embodiment, the prepared samarium-iron-cobalt-phosphorus amorphous thin film contains Sm, Fe, Co and P, wherein the weight ratio of each element is Sm: fe: co: p25: 55: 18: 2, the film thickness is 50 μm.
Comparative example 1
A preparation method of a samarium-iron-cobalt-phosphorus amorphous film comprises the following steps:
(1) activating an electrode slice:
the positive electrode is a platinum electrode plate, the platinum electrode plate is soaked by adopting a mixed solution of acetone and ethanol, the volume fraction of the mixed solution of acetone and ethanol is 75 percent by volume, the soaking time is 5min, and then the platinum electrode plate is dried.
The cathode material is a tungsten sheet with the purity of not less than 99.9 percent, and the tungsten sheet is soaked by mixed solution of acetone and hydrochloric acid, wherein in the mixed solution of acetone and hydrochloric acid, the volume fraction of acetone is 80 percent by volume, the soaking time is 1min, and then the tungsten sheet is dried.
The drying process is carried out in Ar atmosphere at 60 ℃ for 5 min.
(2) Preparing the samarium iron cobalt phosphorus amorphous film by electrochemical codeposition:
heating the electroplating solution to 40 deg.C, pH 4.0, distance between positive and negative electrodes 2.5cm, and current density 4.1A/dm2And the codeposition time is 30min, and the samarium-iron-cobalt-phosphorus amorphous film is obtained.
Wherein the electroplating solution comprises the following components in percentage by mass: 20g/L of phosphoric acid, 15g/L of boric acid, 12g/L of complexing agent, 8g/L of additive, 15g/L of iron salt, 30g/L of samarium salt and 7.5g/L of cobalt salt; comparative example 1 no complexing agent was added, the iron salts were ferric chloride and ferrous sulfate, the total mass concentration of the iron salts was 15g/L, and the mass concentration ratio of ferric chloride to ferrous sulfate was 1: 2; the cobalt salt is cobalt chloride; the samarium salt is samarium chloride hexahydrate, the additives are sodium chloride and potassium chloride, and the mass concentration of the sodium chloride and the potassium chloride is 1: 1, the total mass concentration of the additive is 8 g/L.
(3) Cleaning a film:
and cleaning the samarium-iron-cobalt-phosphorus amorphous film by adopting ultrasonic waves and ethanol, wherein the ultrasonic cleaning time is 3 min.
TABLE 1 preparation conditions and film thicknesses for thin films prepared in examples 1 to 3 and comparative example 1
Table 2 elemental composition of films prepared in examples 1-3 and comparative example 1
As can be seen from tables 1 and 2, the preparation method of the invention can realize the codeposition of the ternary alloy of Sm, Fe and Co, while the Sm content is extremely low by adopting the traditional method, and the Sm content is lower in comparative example 1 because no complexing agent is added.
FIG. 1(a) shows the results of the measurement of the waviness of the surface of the thin film, from which it can be seen that the surface state of the thin film is controllable. FIG. 1(b), (c) and (d) are element scans of Sm, Fe and Co elements, from which it is clear that the amorphous thin film elements are uniformly distributed.
FIG. 2 shows the X-ray diffraction results of the amorphous thin film prepared in example 1, and it can be seen from FIG. 2 that the thin film prepared in the present invention is amorphous.
Fig. 3 is a demagnetization curve of amorphous thin films prepared in example 1 and comparative example 1, wherein the abscissa is: the magnitude of an external magnetic field, and the ordinate is magnetic moment; as can be seen from FIG. 3, after the Co-deposition of three elements Sm, Fe and Co is realized, the saturation magnetization of the amorphous film is 137emu/g, and the saturation magnetization of the amorphous film in comparative example 1 is 125 emu/g.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A samarium iron cobalt phosphorus amorphous film is characterized by comprising Sm, Fe, Co and P, wherein the weight percentage ratio of each element is Sm: fe: co: p ═ x: y: z: a, x is more than or equal to 5.0 and less than or equal to 35.0, y is more than or equal to 55.0 and less than or equal to 80.0, z is more than or equal to 0 and less than or equal to 30.0, a is more than or equal to 0.1 and less than or equal to 2.0, and x + y + z + a is equal to 100.
2. A preparation method of a samarium iron cobalt phosphorus amorphous film, which is characterized by being used for preparing the samarium iron cobalt phosphorus amorphous film in claim 1, and comprising the following steps:
(1) activating an electrode slice:
the positive electrode is a platinum electrode plate, the platinum electrode plate is soaked in a mixed solution of acetone and ethanol for 5-15 min, and then the platinum electrode plate is dried;
the cathode material is tungsten or tantalum slice, soaking for 1-3 min by adopting a mixed solution of acetone and hydrochloric acid, and then drying;
(2) electrochemical co-deposition:
heating the electroplating solution to 40-80 ℃, wherein the pH value is 3.2-5.1, the distance between the anode and the cathode is 2-5 cm, and the current density is 0.5-1.2A/dm2The codeposition time is 10-45 min;
(3) cleaning a film:
ultrasonic wave and ethanol cleaning are adopted to obtain the samarium-iron-cobalt-phosphorus amorphous film.
3. The method for preparing the samarium-iron-cobalt-phosphorus amorphous film according to claim 2, wherein in the step (1), the volume fraction of acetone in the mixed solution of acetone and ethanol is 75-95%; in the mixed solution of acetone and hydrochloric acid, the volume fraction of acetone is 90-98%.
4. The method for preparing the samarium-iron-cobalt-phosphorus amorphous film according to claim 2, wherein in the step (1), the drying is carried out in an Ar atmosphere at a temperature of 50-100 ℃ for 5-12 min.
5. The method for preparing the samarium-iron-cobalt-phosphorus amorphous film according to claim 2, wherein in the step (2): the plating solution comprises, by mass: 5-30g/L of phosphoric acid, 10-20 g/L of boric acid, 2-18 g/L of complexing agent, 3-8 g/L of additive, 10-25 g/L of iron salt, 12-40 g/L of samarium salt and 3-11 g/L of cobalt salt.
6. The method for preparing the samarium-iron-cobalt-phosphorus amorphous film according to claim 5, wherein the complexing agent is: at least one of aminocycloacid, glycine, arginine, ethylene glycol, benzene ring acid, citric acid and tartaric acid.
7. The method of claim 5, in which the ferric salt is at least one of ferric chloride, ferrous sulfate, ferric nitrate, ferrous chloride tetrahydrate, and ferrous nitrate.
8. The method for preparing the samarium-iron-cobalt-phosphorus amorphous film according to claim 5, wherein the cobalt salt is one or both of cobalt chloride and cobalt nitrate.
9. The method of claim 5 in which the samarium salt is at least one of samarium chloride hexahydrate, anhydrous samarium chloride and samarium nitrate.
10. The method of claim 5, wherein the additive is at least one of sodium chloride, potassium chloride, sodium hypochlorite and sodium hypophosphite.
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