CN103184393B

CN103184393B - The preparation method that Nd-Fe-Co-Al is series massive amorphous

Info

Publication number: CN103184393B
Application number: CN201110459419.XA
Authority: CN
Inventors: 郭丽君; 吴学邦; 朱震刚
Original assignee: Hefei Institutes of Physical Science of CAS
Current assignee: Hefei Institutes of Physical Science of CAS
Priority date: 2011-12-28
Filing date: 2011-12-28
Publication date: 2016-02-03
Anticipated expiration: 2031-12-28
Also published as: CN103184393A

Abstract

The preparation method that Nd-Fe-Co-Al is series massive amorphous, relates to non-crystalline material preparing technical field, it is characterized in that: silica tube alloy being put into an end closure, uses B ₂o ₃as alloy purification agent, in mixture of ice and water of being quenched by alloy when continuing to vacuumize, prepare N _d60+X-Y-Zfe _30-Xco _yal _10+Z(wherein 0≤X≤30,0≤Y≤30,0≤Z≤20, and 60+X-Y-Z>=50, X, Y and Z are atomic percent) large block amorphous.Preparation method of the present invention has the feature of its uniqueness: one is put into B in alloy ₂o ₃, the oxide compound of each element can be drawn during fusing, purification alloy, prevent the heterogeneous forming core of alloy from forming crystal, carry heavy alloyed amorphous formation ability; On the other hand because this process continues to vacuumize, can eliminate alloy intrinsic or the pore that melts stylish generation; By regulation and control rate of cooling, control amorphous magnetic property strong and weak.

Description

The preparation method that Nd-Fe-Co-Al is series massive amorphous

Technical field

The present invention relates to non-crystalline material preparing technical field, be specifically related to the preparation method that a kind of Nd-Fe-Co-Al is series massive amorphous.

Background technology

Over nearly more than 20 years, the discovery of Nd-Fe-Al system and Nd-Fe-Co-Al system bulk-metallic glass causes the extensive concern of people, because these bulk-metallic glass systems have the feature being different from other bulk-metallic glass system.One is on thermal analysis curve, do not observe the thermo-negative reaction that glass transition causes, and namely can not clearly determine its second-order transition temperature; Another feature is that this material presents obvious hard magnetic feature when room temperature, and coercive force is about 300KAm ^-1.Research finds that the magnetic of this material and its composition and rate of cooling are closely related, when it is amorphous band, does not show hard magnetic; If when adopting copper mold casting, acquisition large block amorphous, have stronger hard magnetic, size is larger, and hard magnetic is stronger.The preparation method then with large block amorphous is closely bound up for rate of cooling, and therefore, preparation method is one of key element determining Nd base amorphous magnetic property.

At present, the main method for the based bulk amorphous preparation of Nd is copper mold negative pressure casting method.Although the method can reach very high rate of cooling, be conducive to the formation of more large size amorphous block, operation inconvenience, can not add alloy purification agent, and equipment more complicated and costliness.

Summary of the invention

Technical problem to be solved by this invention is to provide a kind of simple to operation, and cost is low, prepares effective large block amorphous preparation method.

Technical problem to be solved by this invention realizes by the following technical solutions.

The preparation method that Nd-Fe-Co-Al is series massive amorphous, is characterized in that: its method steps is,

1. the bulk amorphous alloy size required for reality and atom ratio calculate the weight of each element of Nd, Fe, Co and Al;

2. take Nd, Fe, Co and Al with high Accuracy Electronic Balance, put it in quartz crucible, suction is 10 ^-2more than Pa seals, and inserts in induction furnace and is heated to 800-1000 DEG C, (reference temperature bottom quartz crucible), is incubated air cooling after 5-15 minute and, to room temperature, repeatedly prepares Nd-Fe-Co-Al alloy 3 times;

3. get alloy part in step 2 and put into that internal diameter is 1-10mm (internal diameter can be changed as required), wall thickness is the silica tube of 0.1-2mm, put into appropriate B ₂o ₃, suction to 10 ^-2start after more than Pa to heat up, continue to vacuumize in temperature-rise period, be heated to when temperature is 800-1000 DEG C and be incubated 5-15 minute;

4. the silica tube being placed with alloy melt is put into mixture of ice and water or other cooling material fast, after waiting cooling completely, take out silica tube, break silica tube gently into pieces and obtain cylindrical sample.

The invention has the beneficial effects as follows:

1. B is put in alloy ₂o ₃, the oxide compound of each element can be drawn during fusing, purification alloy, prevent the heterogeneous forming core of alloy from forming crystal, carry heavy alloyed amorphous formation ability;

2. because this process continues to vacuumize, can eliminate alloy intrinsic or the pore that melts stylish generation;

3. by regulation and control rate of cooling (change cooling material or wall thickness of quartz tube thus change temperature), amorphous magnetic property is controlled strong and weak.

Accompanying drawing explanation

Fig. 1 is sample XRD figure spectrum prepared by the present invention;

Fig. 2 is that sample composition EDX prepared by the present invention can spectrogram.

Embodiment

The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific examples, setting forth the present invention further.

Large block amorphous Nd _60+X-Y-Zfe _30-Xco _yal _10+Zpreparation method

(wherein 0≤X≤30,0≤Y≤30,0≤Z≤20, and 60+X-Y-Z >=50, X, Y and Z are atomic percent),

Such as prepare Nd ₆₀fe ₂₀co ₁₀al ₁₀(atm%) large block amorphous, its method steps is,

1. by total amount be 15g calculate, according to Nd ₆₀fe ₂₀co ₁₀al ₁₀(atm%) weight that atom ratio calculates Nd, Fe, Co and Al tetra-kinds of elements is respectively 12.212g, 1.576g, 0.832g and 0.381g;

2. take 12.212gNd, 1.576gFe, 0.832gCo and 0.381gAl put it into an end closure and grow for 500mm, diameter are the silica tube of 12mm, and take the B of 10g ₂o ₃powder puts into silica tube;

3. be refinement silica tube in 300mm place with oxyhydrogen flame at distance silica tube closed port, until the thinnest place of caliber is about 1mm, by refinement, the silica tube the other end that sample is housed to be connected with vacuum pump set and to vacuumize, when in managing, vacuum tightness is 0.01Pa, seal with oxyhydrogen flame;

4. the silica tube of sealing is inserted in induction furnace and be heated to 950 DEG C (reference temperatures bottom quartz crucible), be incubated air cooling room temperature after 10 minutes, repeatedly prepare Nd 3 times ₆₀fe ₂₀co ₁₀al ₁₀alloy;

5. the silica tube that internal diameter is 3mm, wall thickness is 0.8mm and grow for 200mm put into by the alloy taking 4g, puts into the B of 2g ₂o ₃, suction to 10 ^-2start after Pa to heat up, continue to vacuumize in temperature-rise period, be heated to when temperature is 900 DEG C and be incubated 10 minutes;

6. the silica tube being placed with alloy melt is put into bung diameter fast and be about 300mm, height is about 400mm and bucket is about the mixture of ice and water (frozen water volume is about 2: 1) 5 minutes of 350mm built with the degree of depth, breaks silica tube gently into pieces and obtains the column amorphous sample that diameter is about 3mm.

X-ray diffraction (XRD) is done to the sample prepared by above-mentioned steps, judges whether it is non-crystalline material.Fig. 1, Fig. 2, give N _d60fe ₂₀co ₁₀al ₁₀the X-ray diffractogram of (atomic percent) alloy and composition energy spectrogram, XRD figure spectrum presents typical non-crystal structure, does not have sharp-pointed diffraction peak, only has broad peak and time broad peak.

More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.

Claims

The preparation method that 1.Nd-Fe-Co-Al is series massive amorphous, is characterized in that: its method steps is,

A. the bulk amorphous alloy size required for reality and atom ratio calculate the weight of each element of Nd, Fe, Co and Al, and the moiety of this amorphous is N _d60+X-Y-Zfe _30-Xco _yal _10+Z, wherein 0≤X < 30,0 < Y≤30,0≤Z≤20, and 60+X-Y-Z>=50, X, Y and Z are atomic percent;

B. take Nd, Fe, Co and Al with high Accuracy Electronic Balance, put it in quartz crucible, suction is 10 ^-2more than Pa seals, and inserts in induction furnace and is heated to 800-1000 DEG C, is incubated air cooling room temperature after 5-15 minute, repeatedly prepares Nd-Fe-Co-Al alloy more than 3 times;

C. get alloy part in step b and put into that internal diameter is 1-10mm, wall thickness is the silica tube of 0.1-2mm, put into appropriate B ₂o ₃, suction to 10 ^-2start after more than Pa to heat up, continue to vacuumize in temperature-rise period, be heated to when temperature is 800-1000 DEG C and be incubated 5-15 minute;

D. the silica tube being placed with alloy melt is put into mixture of ice and water or other cooling material fast, after waiting cooling completely, take out silica tube, break silica tube gently into pieces and obtain cylindrical sample.