CN103184393A

CN103184393A - Preparation method of Nd-Fe-Co-Al bulk metallic glass

Info

Publication number: CN103184393A
Application number: CN201110459419XA
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: 2013-07-03
Anticipated expiration: 2031-12-28
Also published as: CN103184393B

Abstract

The invention provides a preparation method of Nd-Fe-Co-Al bulk metallic glass. The preparation method is characterized in that alloy is put in a sealed quartz tube, B2O3 is adopted as an alloy scavenging agent, and the alloy is quenched in an ice-water mixture during continuous vacuum-pumping so as to prepare Nd60+X-Y-ZFe30-XCoYAl10+Z bulk metallic glass, wherein X is greater than or equal to 0 and less than or equal to 30, Z is greater than or equal to 0 and less than or equal to 20, 60+X-Y-Z is greater than or equal to 50, and X, Y and Z are all atomic percent. The preparation method provided by the invention has the unique advantages as follows: firstly, B2O3 is put in the alloy and can absorb oxide of each element during melting to scavenge the alloy to prevent the alloy from crystallization of heterogeneous nucleation and improve the glass forming capability of the alloy; secondly, as continuous vacuum-pumping is performed in the process, inherent air holes of the alloy or air holes formed in the alloy during melting can be eliminated; and lastly, the strength of magnetic performance of the glass is controlled through regulation or control of the cooling rate.

Description

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

Technical field

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

Background technology

Over nearly more than 20 years, Nd-Fe-Al system and Nd-Fe-Co-Al are that the discovery of bulk-metallic glass causes people's extensive concern, because these bulk-metallic glass systems have the feature that is different from other bulk-metallic glass system.The one, do not observe the thermo-negative reaction that glass transition causes at thermal analysis curve, namely can not clearly determine its second-order transition temperature; Another characteristics are that this material presents tangible hard magnetic feature when room temperature, and coercive force is about 300KAm ^-1Discover that the magnetic of this material and its composition and rate of cooling are closely related, when it is amorphous band, do not show hard magnetic; If when adopting copper mold casting, that obtains large block amorphously then has a stronger hard magnetic, and size is more big, and hard magnetic is more strong.Rate of cooling is then closely bound up with the Peparation of Bulk Amorphous Solid method, and therefore, the preparation method is one of key element that determines Nd base amorphous magnetic property.

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

Summary of the invention

It is a kind of simple to operation that technical problem to be solved by this invention is to provide, and cost is low, prepares effective Peparation of Bulk Amorphous Solid 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. calculate the weight of Nd, Fe, Co and each element of Al according to the needed bulk amorphous alloy size of reality and atom proportioning;

2. take by weighing Nd, Fe, Co and Al with the high-precision electronic balance, put it in the quartz crucible, suction is 10 ^-2The above sealing of Pa is inserted the induction furnace internal heating to 800-1000 ℃, and (reference temperature of quartz crucible bottom) is incubated after 5-15 minute air cooling and prepares the Nd-Fe-Co-Al alloy 3 times repeatedly to room temperature;

3. getting in the step 2 alloy part, to put into internal diameter be that 1-10mm (internal diameter can be changed as required), wall thickness are the silica tube of 0.1-2mm, puts into an amount of B ₂O ₃, suction to 10 ^-2Begin to heat up after Pa is above, in temperature-rise period, continue to vacuumize, be heated to when temperature is 800-1000 ℃ and be incubated 5-15 minute;

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

The invention has the beneficial effects as follows:

1. put into B in the alloy ₂O ₃, can draw the oxide compound of each element during fusing, purify alloy, prevent that the heterogeneous forming core of alloy from forming crystal, improves the amorphous formation ability of alloy;

2. because this process is to continue to vacuumize, can eliminate alloy pore intrinsic or that melt stylish generation;

3. by regulation and control rate of cooling (thereby changing cooling material or wall thickness of quartz tube change temperature), control amorphous magnetic property power.

Description of drawings

Fig. 1 is the sample XRD figure spectrum of the present invention's preparation;

Fig. 2 can spectrogram for the sample composition EDX of the present invention's preparation.

Embodiment

For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with specific examples, further set forth the present invention.

Large block amorphous Nd _60+X-Y-ZFe _30-XCo _YAl _10+ZThe preparation method

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

For example prepare Nd ₆₀Fe ₂₀Co ₁₀Al ₁₀(atm%) large block amorphous, its method steps is,

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

2. taking by weighing 12.212g Nd, 1.576g Fe, 0.832g Co and 0.381g Al puts it into an end closure and long be the silica tube of 12mm, and take by weighing the B of 10g for 500mm, diameter ₂O ₃Powder is put into silica tube;

3. be refinement silica tube in 300mm place with oxyhydrogen flame at distance silica tube closed port, the thinnest place is about 1mm until caliber, refinement, that sample is housed the silica tube the other end is connected with the vacuum unit vacuumizes, when vacuum tightness is 0.01Pa in the pipe, seal with oxyhydrogen flame;

4. the silica tube of sealing is inserted induction furnace internal heating to 950 ℃ (reference temperature of quartz crucible bottom), be incubated air cooling room temperature after 10 minutes, prepare Nd 3 times repeatedly ₆₀Fe ₂₀Co ₁₀Al ₁₀Alloy;

5. it is that 3mm, wall thickness are 0.8mm and longly are the silica tube of 200mm that the alloy that takes by weighing 4g is put into internal diameter, puts into the B of 2g ₂O ₃, suction to 10 ^-2Begin behind the Pa to heat up, in temperature-rise period, continue to vacuumize, be heated to when temperature is 900 ℃ and be incubated 10 minutes;

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

To doing X-ray diffraction (XRD) by the sample of above-mentioned steps preparation, judge whether it is non-crystalline material.Fig. 1, Fig. 2 have provided N _D60Fe ₂₀Co ₁₀Al ₁₀The X-ray diffractogram of (atomic percent) alloy and composition energy spectrogram, the XRD figure spectrum presents typical non-crystal structure, does not have sharp-pointed diffraction peak, has only broad peak and time broad peak.

More than show and described 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; that describes in above-described embodiment and the 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.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims

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

A. calculate the weight of Nd, Fe, Co and each element of Al according to the needed bulk amorphous alloy size of reality and atom proportioning;

B. take by weighing Nd, Fe, Co and Al with the high-precision electronic balance, put it in the quartz crucible, suction is 10 ^-2The above sealing of Pa is inserted the induction furnace internal heating to 800-1000 ℃, is incubated air cooling room temperature after 5-15 minute, prepares the Nd-Fe-Co-Al alloy repeatedly more than 3 times;

C. get among the step b alloy part and put into silica tube, put into an amount of B ₂O ₃, suction to 10 ^-2Begin to heat up after Pa is above, in temperature-rise period, continue to vacuumize, be heated to when temperature is 800-1000 ℃ and be incubated 5-15 minute;

The silica tube that d. will be placed with alloy melt is put into mixture of ice and water or other cooling material fast, wait fully cooling after, take out silica tube, break silica tube gently into pieces and obtain cylindrical sample.

2. the series massive amorphous preparation method of Nd-Fe-Co-Al according to claim 1, it is characterized in that: the frozen water volume of described mixture of ice and water is 2: 1.

3. Peparation of Bulk Amorphous Solid method according to claim 1, it is characterized in that: the internal diameter of described silica tube is that 1-10mm, wall thickness are 0.1-2mm.