CN104862618B - A kind of composite amorphous magnetically soft alloy material and preparation method thereof - Google Patents

Abstract

A method for preparing a composite amorphous soft magnetic alloy material, the composition of the composite amorphous soft magnetic alloy material is Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ ‑Ni ₇₁ P ₂₉ ; the preparation method is as follows: first prepare an amorphous soft magnetic alloy thin Then prepare the electroless nickel-phosphorus plating solution and prepare composite amorphous soft magnetic alloy by chemical deposition method. The advantages of the present invention are: the compound amorphous soft magnetic alloy prepared by the chemical deposition method of the present invention has superior performance: the initial magnetic permeability can be improved in the range of frequency 1kHz-1MHz and the condition of alternating magnetic field of 0.05A/m An order of magnitude, which remains basically constant at 1870; its relaxation frequency and quality factor are significantly improved compared with the original alloy. The invention has simple process, convenient operation and low cost, and is suitable for large-scale batch industrial production.

Description

A kind of composite amorphous soft magnetic alloy material and preparation method thereof

technical field

The invention relates to the field of magnetic functional soft magnetic materials and chemical deposition of nickel phosphorus, in particular to a composite amorphous soft magnetic alloy material and a preparation method thereof.

Background technique

Soft magnetic materials refer to those metal magnetic materials with low coercive force and high magnetic permeability, which have important and extensive applications in electricity, electronics and modern new technologies. With the rapid development of digital communication technology and optical fiber communication, traditional analog communication equipment is constantly updated and eliminated; most of the various power transformers used in the communication field work at low magnetic flux density, and the magnetic permeability of the material starts at this time. played a major role. Especially with the development of high-frequency technology, higher requirements are put forward for the high-frequency characteristics of soft magnetic materials. Magnetic permeability is one of the basic parameters of soft magnetic materials. It mainly refers to the initial magnetic permeability μ _i , which is the magnetic permeability of the material whose working point is at the initial part of the magnetization curve. For soft magnetic materials applied under weak magnetic fields, this is The most important performance indicator. However, high permeability materials should not only have high initial permeability, but also have high quality factor, high relaxation frequency, etc., and today's iron-nickel alloys often pursue high permeability at the same time. Ignoring this part of the requirements, it is impossible to take into account other parameters while improving the magnetic permeability, so that the material properties can reach a good balance.

The relaxation frequency f ₀ and quality factor Q of soft magnetic alloys are two important parameters to evaluate their high-frequency performance. Higher relaxation frequency and larger quality factor indicate that the material has better high-frequency performance. Under alternating magnetic field conditions, it is desirable to maintain the high initial permeability of the material at low frequencies to higher frequencies. Therefore, soft magnetic alloys with high initial permeability that can be applied under high-frequency conditions must be widely used.

Electroless plating is a suitable method for preparing soft magnetic coatings by wet method. Compared with the mature electroplating industry, electroless plating has its unique advantages: low price, simple preparation method, no external power supply, power transmission system and auxiliary electrodes, and only need to hang the workpiece in the plating solution correctly during operation; The coating is relatively uniform, and can be evenly plated on complex-shaped substrates; it can be plated on non-conductive substrates; it is plated by the self-catalytic activity of the substrate, so the bonding force is generally better than electroplating; the coating is dense and the porosity is low. And electroless Ni-P plating has soft magnetic properties comparable to electroplating.

Contents of the invention

The purpose of the present invention is to provide a composite amorphous soft magnetic alloy material and a preparation method thereof for the above-mentioned technical analysis and existing problems. The composite amorphous soft magnetic alloy material still has a high initial magnetic permeability at relatively high frequencies. At the same time, it has a higher quality factor and relaxation frequency.

Technical scheme of the present invention:

A composite amorphous soft magnetic alloy material, the composition is Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ -Ni ₇₁ P ₂₉ .

A preparation method of the composite amorphous soft magnetic alloy material, the steps are as follows:

1) Preparation of master alloy ingot

Fe, Co, Si, and B raw materials with a purity of not less than 99.9% are selected respectively, and ingredients are prepared according to the mass percentage of elements, and melted into Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ master alloy ingots in a vacuum induction furnace, and the weight loss is controlled to be no more than 5%. ;

2) Preparation of Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous alloy ribbon

The Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous soft magnetic alloy thin strip sample was prepared in the atmosphere by the single-roller melt rotation quenching method. The width of the amorphous thin strip is 22mm and the thickness is 25.2μm;

3) Pretreatment of Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous alloy ribbon

Under room temperature and external ultrasonic conditions, soak the above-mentioned amorphous strip in absolute ethanol solution for 20 minutes, take it out and rinse it with deionized water three times to remove surface oil, adsorbed impurities and loose oxides on the surface;

4) Preparation of electroless nickel-phosphorus plating solution

The electroless nickel phosphorus plating solution is a mixed solution made of nickel sulfate, sodium hypophosphite, sodium citrate, lactic acid and anhydrous sodium acetate dissolved in distilled water. The concentration of each component in the mixed solution is: nickel sulfate 25g/ L, sodium hypophosphite 40g/L, sodium citrate 10g/L, lactic acid 15ml/L, anhydrous sodium acetate 30g/L, the mixed solution is adjusted to be 4.4-4.6 by adding anhydrous sodium carbonate;

5) Preparation of Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ -Ni ₇₁ P ₂₉ composite soft magnetic alloy material

The Ni ₇₁ P ₂₉ magnetic layer was deposited on the Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous soft magnetic alloy. The method was as follows: the pretreated amorphous strip was placed in the prepared electroless nickel-phosphorus plating solution, and the Plating was carried out at 86-88°C for 10 minutes under agitation. After taking it out, it was rinsed three times with deionized water and air-dried to obtain Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ -Ni ₇₁ P ₂₉ composite amorphous soft magnetic alloy.

Advantage and beneficial effect of the present invention are:

The composite amorphous soft magnetic alloy prepared by the chemical deposition method has excellent high-frequency performance, and its relaxation frequency is as high as 5.11MHz; its quality factor is 12 under the condition of 1MHz; the magnetic field is 0.05A/ in the frequency range of 1kHz-1MHz Under the condition of m, the initial magnetic permeability remains basically constant at 1870; the invention has simple process, convenient operation and low cost, and is suitable for large-scale batch industrial production.

detailed description

Example:

A method for preparing a composite amorphous soft magnetic alloy material. The composition of the composite amorphous soft magnetic alloy material is Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ -Ni ₇₁ P ₂₉ , which is prepared by chemical deposition. The steps are as follows:

1) Preparation of master alloy ingot

Fe, Co, Si, and B raw materials with a purity of 99.95% were respectively selected, and ingredients were prepared according to the mass percentage of the elements, and melted into Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ master alloy ingots in a vacuum induction furnace, and the weight loss was controlled to 4%;

2) Preparation of Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous alloy ribbon

The Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous soft magnetic alloy thin strip sample was prepared in the atmosphere by the single-roller melt rotation quenching method. The width of the amorphous thin strip is 22mm and the thickness is 25.2μm;

3) Pretreatment of Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous alloy ribbon

Under room temperature and external ultrasonic conditions, soak the above-mentioned amorphous strip in absolute ethanol solution for 20 minutes, take it out and rinse it with deionized water three times to remove surface oil, adsorbed impurities and loose oxides on the surface;

4) Preparation of electroless nickel-phosphorus plating solution

The electroless nickel phosphorus plating solution is a mixed solution made of nickel sulfate, sodium hypophosphite, sodium citrate, lactic acid and anhydrous sodium acetate dissolved in distilled water. The concentration of each component in the mixed solution is: nickel sulfate 25g/ L, sodium hypophosphite 40g/L, sodium citrate 10g/L, lactic acid 15ml/L, anhydrous sodium acetate 30g/L, the mixed solution is adjusted to be 4.4-4.6 by adding anhydrous sodium carbonate;

5) Preparation of Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ -Ni ₇₁ P ₂₉ composite soft magnetic alloy material

The Ni ₇₁ P ₂₉ magnetic layer was deposited on the Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous soft magnetic alloy. The method was as follows: the pretreated amorphous strip was placed in the prepared electroless nickel-phosphorus plating solution, and the Plating was carried out for 10 minutes at 86°C under stirring conditions, and after taking it out, it was rinsed with deionized water three times and air-dried to obtain Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ -Ni ₇₁ P ₂₉ composite amorphous soft magnetic alloy. The thickness of the amorphous ribbon is 26.7 μm.

Table 1 shows the initial permeability of Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ amorphous soft magnetic alloy and Fe ₆₇ Co ₁₈ Si ₁₁ B ₄ -Ni ₇₁ P ₂₉ composite soft magnetic alloy at a frequency of 1kHz and a magnetic field of 0.05A/m The rate μ, the relaxation frequency f ₀ , and the quality factor Q at 1MHz.

Table 1

Claims (2)

1. a kind of composite amorphous magnetically soft alloy material, it is characterised in that：Composition is Fe₆₇Co₁₈Si₁₁B₄-Ni₇₁P₂₉。

2. a kind of preparation method of composite amorphous magnetically soft alloy material as claimed in claim 1, it is characterised in that step is as follows：

1) preparation of master alloy ingot

Fe, Co, Si, B raw material that purity is not less than 99.9% are chosen respectively, dispensing are carried out according to element mass percent, true Fe is smelted into empty induction furnace₆₇Co₁₈Si₁₁B₄Master alloy ingot, control is weightless to be no more than 5%；

2)Fe₆₇Co₁₈Si₁₁B₄The preparation of amorphous alloy ribbon

Fe is prepared using single roller melt rotation quick quenching technique in an atmosphere₆₇Co₁₈Si₁₁B₄Amorphous soft magnetic ribbon sample, amorphous is thin The width of band is that 22mm, thickness are 25.2 μm；

3)Fe₆₇Co₁₈Si₁₁B₄The pretreatment of amorphous alloy ribbon

Under the conditions of room temperature and outer ultrasonic ripple, above-mentioned amorphous thin ribbon is placed in ethanol solution and soaks 20min, is used after taking-up Deionized water elutes the oxide of three greasy dirts to remove surface, the impurity of absorption and surface porosity；

4) preparation of chemical nickel plating phosphor bath

Chemical nickel plating phosphor bath is to be dissolved in aquae destillata system by nickel sulfate, sodium hypophosphite, sodium citrate, lactic acid and anhydrous sodium acetate Into mixed liquor, the concentration of each component is in mixed liquor：Nickel sulfate 25g/L, sodium hypophosphite 40g/L, sodium citrate 10g/L, Lactic acid 15ml/L, anhydrous sodium acetate 30g/L, mixed liquor are 4.4-4.6 by adding natrium carbonicum calcinatum to adjust pH value；

5)Fe₆₇Co₁₈Si₁₁B₄-Ni₇₁P₂₉The preparation of composite soft magnetic alloy material

In Fe₆₇Co₁₈Si₁₁B₄Ni is carried out on amorphous soft-magnetic alloy₇₁P₂₉Magnetospheric deposition, method is as follows：By by pretreatment Amorphous thin ribbon is placed in the chemical nickel plating phosphor bath of preparation, is used under 86-88 DEG C of temperature, stirring condition after plating 10min, taking-up Deionized water is eluted three times, natural air drying, and Fe is made₆₇Co₁₈Si₁B₁₄-Ni₇₁P₂₉Composite amorphous magnetically soft alloy.