CN104328367A - Method for preparing ribbon amorphous alloy under mild condition - Google Patents

Method for preparing ribbon amorphous alloy under mild condition Download PDF

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Publication number
CN104328367A
CN104328367A CN201410564957.9A CN201410564957A CN104328367A CN 104328367 A CN104328367 A CN 104328367A CN 201410564957 A CN201410564957 A CN 201410564957A CN 104328367 A CN104328367 A CN 104328367A
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amorphous alloy
amorphous metal
crystaline amorphous
pet
film
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CN201410564957.9A
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CN104328367B (en
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傅雅琴
钱晨
傅强
俞璐军
赵永振
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Zhejiang Sci Tech University ZSTU
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Zhejiang Sci Tech University ZSTU
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Abstract

The invention discloses a method for preparing a ribbon amorphous alloy under a mild condition. A ribbon polyester (PET) film is used as a base material, and a nickel-cobalt-iron-phosphorus amorphous alloy coating is plated on the surface of the PET film; the method comprises the steps of coating and plating the amorphous alloy and removing the film; particularly, the method comprises the steps of soaking the PET film with alkali weigh reduction on one side in SnCl2 and PdCl2 liquids with set concentrations sequentially for a certain time, then soaking in a mixed liquid of Na3C6H5O7, H3BO3, Na2H2PO2, NiSO4, CoSO4, and FeSO4, wherein the mixed liquid with certain concentration and certain pH value is at certain temperature, coating the amorphous alloy coating on the PET film, and carrying out accelerant-containing alkaline liquid treatment, superheated steam treatment and 350-450 DEG C heat treatment to obtain the ribbon amorphous alloy. The process is simple and effective, the preparation condition is mild, and the ribbon amorphous alloy can be effectively prepared.

Description

A kind of method preparing banded non-crystaline amorphous metal in a mild condition
Technical field
The present invention relates to the preparation method of non-crystaline amorphous metal, particularly relate to a kind of method preparing banded non-crystaline amorphous metal in a mild condition.
Background technology
Non-crystaline amorphous metal refers to using metallic bond as its constitutional features, is topological disorder shape in three-dimensional atomic arrangement, does not have the crystal grain of crystal alloy, crystal boundary.Compared with the crystal alloy of routine, non-crystaline amorphous metal has excellent mechanical property (high strength, high rigidity etc.), magnetic, solidity to corrosion, wear resistance, high resistivity and the advantage such as electromechanical coupling performance and hydrogen storage property, machinery, communication, electric power, aerospace, automotive industry and even national defense and military all have a wide range of applications potentiality.What the preparation of non-crystaline amorphous metal adopted usually is super quench solidification, and namely usually require high temperature and high speed of cooling, the setting time of alloy is extremely short, is difficult to control.Harsh owing to preparing required condition, need to cool rapidly with the speed of 1,000,000 degree per second, make production cost higher, and due to the impact by cooling rate, be difficult to produce the amorphous alloy strips of thickness more than 50 microns, affect large-scale commercial applications.Therefore, utilize the method for simple possible to produce thickness in a mild condition and the method for amorphous alloy strips more than 50 microns can have great realistic meaning.
Summary of the invention
The object of the invention is for condition required in conventional non-crystaline amorphous metal preparation process harsh, and be difficult to prepare thickness amorphous alloy strips problem more than 50 microns, provide a kind of method preparing banded non-crystaline amorphous metal in a mild condition.
The object of the invention is to be achieved through the following technical solutions, a kind of method preparing banded non-crystaline amorphous metal in a mild condition, comprises the following steps:
(1) by one side alkali mass loss rate be banded polyester (PET) film of 5%-15%, successively at the SnCl of 10-15g/L 2the PdCl of 5-10 min, 0.15-0.30g/L is soaked in solution (room temperature) 2solution (room temperature) middle immersion 5-10 min, temperature are 50-60 DEG C, pH value is soak 2.5-3.5 hour in the Ni-Co-Fe mixing solutions of 8.0-8.5, then use the heat water-spraying 5-10 min of 60 DEG C, at 80 DEG C, after dry 30-60 min, obtain band shape (PET) film being coated with non-crystaline amorphous metal; Described SnCl 2solution and PdCl 2the solvent of solution is deionized water; The each component of described Ni-Co-Fe mixing solutions is as follows: 50-70g/L Na 3c 6h 5o 7, 0.5 mol/L H 3bO 3, 20-30g/L Na 2h 2pO 2, 0.04 mol/L NiSO 4, 0.015 mol/L CoSO 4, 0.01-0.02 mol/L FeSO 4, solvent is deionized water;
(2) PET film being coated with non-crystaline amorphous metal is soaked 20-30 min in NaOH and TF1181 mixed aqueous solution, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 5-10g/L, TF1181 is 0.5-1.0 g/L; Then 5 min are sprayed by the hot steam of 120 DEG C, after washing, thermal treatment 5min under the condition of 350-450 DEG C, obtained banded non-crystaline amorphous metal.
The invention has the beneficial effects as follows, banded non-crystaline amorphous metal method prepared by the present invention is simple, processing condition are gentle, and the banded non-crystaline amorphous metal thickness obtained can more than 50 microns, and can regulate and control the thickness of banded amorphous alloy layer by the concentration of each solution and soak time in the solution; And can according to the ratio of mixing solutions, the atomic ratio in regulation and control non-crystaline amorphous metal;
PET is adopted to be base film material in the present invention, after being partly dissolved in containing the NaOH solution of base reduction promoter, under the effect of superheated vapour, pierceability can be formed dissolve, avoid PET makes top layer banded non-crystaline amorphous metal fracture because of high-temperature shrinkage, and thermal treatment certain hour can remove film completely at 350-450 DEG C, obtain the non-au-alloy of pure band shape.
Accompanying drawing explanation
Fig. 1 is the non-crystaline amorphous metal schematic diagram that the present invention obtains on PET film surface;
Fig. 2 is ultimate analysis (EDS) spectrogram of the non-crystaline amorphous metal that embodiment 1 obtains;
Fig. 3 is the X-ray diffractogram of the non-crystaline amorphous metal that embodiment 1 obtains;
Fig. 4 is ultimate analysis (EDS) spectrogram of the non-crystaline amorphous metal that embodiment 2 obtains;
Fig. 5 is the X-ray diffractogram of the non-crystaline amorphous metal that embodiment 2 obtains.
Embodiment
Prepare a method for banded non-crystaline amorphous metal in a mild condition, comprise the following steps:
(1) by one side alkali mass loss rate be banded polyester (PET) film of 5%-15%, successively at the SnCl of 10-15g/L 2the PdCl of 5-10 min, 0.15-0.30g/L is soaked in solution (room temperature, 25 DEG C) 2solution (room temperature, 25 DEG C) in soak 5-10 min, temperature is 50-60 DEG C, pH value is soak 2.5-3.5 hour in the Ni-Co-Fe mixing solutions of 8.0-8.5, then use the heat water-spraying 5-10 min of 60 DEG C, at 80 DEG C, after dry 30-60 min, obtain band shape (PET) film being coated with non-crystaline amorphous metal; Described SnCl 2solution and PdCl 2the solvent of solution is deionized water; The each component of described Ni-Co-Fe mixing solutions is as follows: 50-70g/L Na 3c 6h 5o 7, 0.5 mol/L H 3bO 3, 20-30g/L Na 2h 2pO 2, 0.04 mol/L NiSO 4, 0.015 mol/L CoSO 4, 0.01-0.02 mol/L FeSO 4, solvent is deionized water; This step completes in a mild condition, regulates and controls the thickness of banded amorphous alloy layer by the concentration of each solution and soak time in the solution, and can according to the ratio of mixing solutions, the atomic ratio in regulation and control non-crystaline amorphous metal.
(2) PET film being coated with non-crystaline amorphous metal is soaked 20-30 min in NaOH and TF1181 mixed aqueous solution, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 5-10g/L, TF1181 is 0.5-1.0 g/L; Then spray 5 min by the hot steam of 120 DEG C, PET pierceability is partly dissolved, after washing, at the thermal treatment 5-20 min of 350-450 DEG C, after removing PET film completely, obtained banded non-crystaline amorphous metal.PET is adopted to be base film material in the present invention, after being partly dissolved in containing the NaOH solution of base reduction promoter, under the effect of superheated vapour, pierceability can be formed dissolve, avoid PET makes top layer banded non-crystaline amorphous metal fracture because of high-temperature shrinkage, and thermal treatment certain hour can remove film completely at 350-450 DEG C, obtain the non-au-alloy of pure band shape.
Below in conjunction with embodiment, the invention will be further described.
embodiment 1:
(1) by one side alkali mass loss rate be 5% banded polyester (PET) film, successively at the SnCl of 10g/L 2the PdCl of 10 min, 0.30g/L is soaked in solution (room temperature, 25 DEG C) 2solution (room temperature, 25 DEG C) middle immersion 5 min, temperature is 50 DEG C, pH value is soak 2.5 hours in the Ni-Co-Fe mixing solutions of 8.5, then uses heat water-spraying 5 min of 60 DEG C, obtains band shape (PET) film being coated with non-crystaline amorphous metal at 80 DEG C after dry 30 min; The each component of described Ni-Co-Fe mixing solutions is as follows: 50g/L Na 3c 6h 5o 7, 0.5 mol/L H 3bO 3, 20g/L Na 2h 2pO 2, 0.04 mol/L NiSO 4, 0.015 mol/L CoSO 4, 0.01 mol/L FeSO 4, solvent is deionized water.
(2) PET film being coated with non-crystaline amorphous metal is soaked 20 min in NaOH and TF1181 mixing solutions, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 10g/L, TF1181 is 0.5 g/L; Then spray 5 min by the hot steam of 120 DEG C, PET pierceability is partly dissolved, after washing, enter the tube furnace process 20min of 350 DEG C, after removing PET film completely, obtained thickness is the banded non-crystaline amorphous metal of 50 microns.
The ultimate analysis of products therefrom is as shown in Figure 2, as can be seen from the figure, main containing metallic elements such as Fe, Co, Ni in the product prepared under this condition, and proportionlity is: Fe:Co:Ni=2.02:6.71:69.53.
As shown in Figure 3, as seen from Figure 3, product does not produce diffraction peak to the XRD of products therefrom, illustrates that this product is amorphous.
embodiment 2:
(1) by one side alkali mass loss rate be 15% banded polyester (PET) film, successively at the SnCl of 15g/L 2the PdCl of 5min, 0.15g/L is soaked in solution (room temperature, 25 DEG C) 2solution (room temperature, 25 DEG C) in soak that 10min, temperature are 60 DEG C, pH value is soak 3.5 hours in the Ni-Co-Fe mixing solutions of 8.0, then use the heat water-spraying 10min of 60 DEG C, at 80 DEG C, after dry 60min, obtain band shape (PET) film being coated with non-crystaline amorphous metal; The each component of described Ni-Co-Fe mixing solutions is as follows: 70g/L Na 3c 6h 5o 7, 0.5 mol/L H 3bO 3, 30g/L Na 2h 2pO 2, 0.04 mol/L NiSO 4, 0.015 mol/L CoSO 4, 0.02 mol/L FeSO 4, solvent is deionized water.
(2) PET film being coated with non-crystaline amorphous metal is soaked 30min in NaOH and TF1181 mixing solutions, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, and the solubility of NaOH is the concentration of 5g/L, TF1181 is 1.0 g/L; Then with the hot steam spray 5min of 120 DEG C, PET pierceability is partly dissolved, after washing, enters the tube furnace process 5min of 450 DEG C, after removing PET film completely, obtained thickness is the banded non-crystaline amorphous metal of 85 microns.
The ultimate analysis of products therefrom is as shown in Figure 4, as can be seen from the figure, main containing metallic elements such as Fe, Co, Ni in the product prepared under this condition, and proportionlity is: 2.34:6.77:71.51.
The XRD of products therefrom as shown in Figure 5, as seen from Figure 5, the XRD diffracting spectrum of product and the diffracting spectrum of embodiment 1 products therefrom basically identical, all do not produce diffraction peak, illustrate that this product is amorphous.
Above-described embodiment is used for explaining and the present invention is described, instead of limitation of the present invention, in the protection domain of spirit of the present invention and claim, to any amendment of the present invention and change, all falls into protection scope of the present invention.

Claims (1)

1. prepare a method for banded non-crystaline amorphous metal in a mild condition, it is characterized in that, it comprises the following steps:
(1) by one side alkali mass loss rate be banded polyester (PET) film of 5%-15%, successively at the SnCl of 10-15g/L 2the PdCl of solution soaking 5-10 min, 0.15-0.30g/L 2solution soaking 5-10 min, 2.5-3.5 hour is soaked in the Ni-Co-Fe mixing solutions that temperature is 50-60 DEG C, pH value is 8.0-8.5, then use the heat water-spraying 5-10 min of 60 DEG C, at 80 DEG C, obtain the banded PET film being coated with non-crystaline amorphous metal after dry 30-60 min; The each component of described Ni-Co-Fe mixing solutions is as follows: 50-70g/L Na 3c 6h 5o 7, 0.5 mol/L H 3bO 3, 20-30g/L Na 2h 2pO 2, 0.04 mol/L NiSO 4, 0.015 mol/L CoSO 4, 0.01-0.02 mol/L FeSO 4, solvent is deionized water;
(2) PET film being coated with non-crystaline amorphous metal that step (1) obtains is soaked 20-30 min in NaOH and TF1181 mixing solutions, the temperature of described NaOH and TF1181 mixing solutions is 95 DEG C, the concentration of NaOH solution is the concentration of 5-10g/L, TF1181 is 0.5-1.0 g/L; Then spray 5 min by the hot steam of 120 DEG C, after washing, under the condition of 350-450 DEG C, process 5-20 min, obtained banded non-crystaline amorphous metal.
CN201410564957.9A 2014-10-22 2014-10-22 A kind of method of preparing banded non-crystaline amorphous metal under temperate condition Expired - Fee Related CN104328367B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112250227A (en) * 2020-09-11 2021-01-22 杭州娃哈哈科技有限公司 Zero-emission alkaline electrolyzed water production device

Citations (6)

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Publication number Priority date Publication date Assignee Title
US4368221A (en) * 1980-07-04 1983-01-11 Bacs Megyei Allami Epitoipari Vallalat Process for coating fibrous glass with amorphous nickel phosphorous glass metal
CN1710137A (en) * 2005-06-23 2005-12-21 复旦大学 Amorphous nickel-boron nuclear-shell, ghost structural material and its preparing material
CN1737183A (en) * 2005-07-28 2006-02-22 复旦大学 Process for preparing noncrystalline nickel-phosphor-core - shell, hollow shell structure material
CN1843997A (en) * 2005-04-08 2006-10-11 富士电机电子设备技术株式会社 Method of plating on a glass base plate, a disk substrate, method for manufacturing the same and a perpendicular magnetic recording medium
RU2501888C1 (en) * 2012-07-20 2013-12-20 Федеральное государственное бюджетное учреждение науки институт физики им. Л.В. Киренского Сибирского отделения Российской академии наук METHOD OF PRODUCING AMORPHOUS MAGNETIC Co-P FILMS
CN103632794A (en) * 2012-08-28 2014-03-12 有研稀土新材料股份有限公司 Composite soft magnetic material and method for preparing material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4368221A (en) * 1980-07-04 1983-01-11 Bacs Megyei Allami Epitoipari Vallalat Process for coating fibrous glass with amorphous nickel phosphorous glass metal
CN1843997A (en) * 2005-04-08 2006-10-11 富士电机电子设备技术株式会社 Method of plating on a glass base plate, a disk substrate, method for manufacturing the same and a perpendicular magnetic recording medium
CN1710137A (en) * 2005-06-23 2005-12-21 复旦大学 Amorphous nickel-boron nuclear-shell, ghost structural material and its preparing material
CN1737183A (en) * 2005-07-28 2006-02-22 复旦大学 Process for preparing noncrystalline nickel-phosphor-core - shell, hollow shell structure material
RU2501888C1 (en) * 2012-07-20 2013-12-20 Федеральное государственное бюджетное учреждение науки институт физики им. Л.В. Киренского Сибирского отделения Российской академии наук METHOD OF PRODUCING AMORPHOUS MAGNETIC Co-P FILMS
CN103632794A (en) * 2012-08-28 2014-03-12 有研稀土新材料股份有限公司 Composite soft magnetic material and method for preparing material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112250227A (en) * 2020-09-11 2021-01-22 杭州娃哈哈科技有限公司 Zero-emission alkaline electrolyzed water production device
CN112250227B (en) * 2020-09-11 2022-05-27 杭州娃哈哈科技有限公司 Zero-emission alkaline electrolyzed water production device

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