CN103212714A - Method for preparing neodymium iron boron material - Google Patents
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Abstract
The invention discloses a method for preparing neodymium iron boron material. The method comprises the following operation steps that neodymium iron boron magnetic powder and graphene powder are evenly mixed to form mixed powder, the mixed powder is oriented and pressed in a magnetic filed to prepare blank, and then sintering heat treatment is conducted on the blank to obtain the neodymium iron boron material; the mixed powder comprises, by weight, 0.03-0.20% of the graphene powder, the component of the graphene powder is RwQxMyNz, the R is one kind or a plurality of kinds of Pr, Nd, Dy, Tb, Ho and Gd, the Q is one kind or two kinds of Fe and Co, the M is an element B, and the N is one kind or a plurality of kinds of Al, Nb, Zr, Cu, Ga, Mo, W and V; the w is greater than or equal to 29 and less than or equal to 33, the x is greater than or equal to 60 and less than or equal to 69, the y is greater than or equal to 0.98 and less than or equal to 1.2, the z is greater than or equal to 0 and less than or equal to 3, and the sum of the w, the x, the y and the z is 100. The neodymium iron boron material prepared through the method has small and even grains, and has excellent mechanical properties and coercive force.
Description
Technical field
The present invention relates to the production field of magnet, be specifically related to a kind of method for preparing NdFeB material.
Background technology
The conventional sintering neodymium-iron-boron magnetic material belongs to typical sintered metal product, compression strength is little, fragility greatly, easily cause along brilliant fracture from crystal boundary, along with the continuous expansion in Sintered NdFeB magnet applications field, the test of adverse circumstances such as magnet unavoidably will experience a shock, vibration.In a single day magnet breaks, and will bring massive losses to the user.Therefore must do further investigation to Sintered NdFeB magnet mechanical property, optimize production technology, mechanical properties such as the compression strength of raising magnet, toughness reduce breakage in the blank subsequent processes and the danger of rupturing in environment for use.The basic mechanical design feature index of neodymium-iron-boron magnetic material is coercivity H (comprising HCJ Hcj and magnetic strength coercivity H b), remanent magnetism Br, magnetic energy product (BH) max and Curie temperature Tc.The researcher of neodymium-iron-boron magnetic material and the main task of manufacturer are exactly to develop the potentiality of material to greatest extent, improve coercivity H, remanent magnetism Br, magnetic energy product (BH) max and the Curie temperature Tc of permanent-magnet material.Wherein coercivity is the ability that magnet keeps permanent magnetism, and required opposing magnetic field intensity is measured when generally dropping to zero with the magnetically saturated magnetic induction intensity of material.Coercitive improvement can improve the temperature stability of NdFeB material material.Therefore the coercivity that improves neodymium-iron-boron magnetic material is the tireless pursuit of client and magnet manufacturer.
Goal of the invention
The object of the present invention is to provide a kind of method for preparing NdFeB material, the crystal grain of the NdFeB material that it is prepared is tiny, even, mechanical property and coercivity obviously improve.
Its scheme of taking is specific as follows:
A kind of method for preparing NdFeB material, its operation is as follows: NdFeB magnetic powder and Graphene powder mixing are configured to mixed powder, again mixed powder is orientated and is pressed into blank in magnetic field, then blank is carried out sintering heat treatment and can produce and obtain NdFeB material; The content of Graphene powder is 0.03～0.20wt% in the mixed powder; The composition of described NdFeB magnetic powder is R
wQ
xM
yN
z, wherein R is one or more in Pr, Nd, Dy, Tb, Ho, the Gd element, and Q is one or both in Fe, the Co element, and M is the B element, and N is one or more in Al, Nb, Zr, Cu, Ga, Mo, W, the V element; 29≤w≤33,60≤x≤69,0.98≤y≤1.2,0≤z≤3, w+x+y+z=100.
Because Graphene is a kind of flat film material of the individual layer laminated structure of being made up of with the sp﹠sup2 hybridized orbit carbon atom, its thin thickness, intensity are big, among the present invention, the mixed powder sintering of Graphene powder and NdFeB magnetic powder configuration is made NdFeB material, prepare in the NdFeB material process at sintering, Graphene places Nd-Fe-B alloy crystal boundary place as the item that mixes, and hinders moving of crystal boundary, stop the gathering and the growth of crystal grain, thereby obtain tiny, the uniform NdFeB material of crystal grain.And because Graphene is non magnetic phase alloy, the domain wall during to magnetic reversal moves and can play the effect of nail letter, can effectively hinder moving of domain wall, thereby improve the performances such as coercivity of sintered Nd-Fe-B permanent magnetic material, improves the stability of neodymium-iron-boron magnetic material.In addition, the intensity superelevation of Graphene own also has corresponding raising so added the compression strength and the toughness of the neodymium-iron-boron magnetic material of micro-Graphene preparation.
Can the magnetic property of neodymium-iron-boron magnetic material be had a negative impact owing to carbon element content in addition.So carbon content is carried out strictness restriction and (is controlled generally that carbon content is 300～2500ppm) in the mixed powder in the NdFeB magnetic powder that reply is selected for use, after making that the later stage Graphene adds, the carbon content of the Nd-Fe-B permanent magnetic material of sintering preparation maintains in certain scope, that is carbon content guarantees the magnetic behavior of neodymium-iron-boron magnetic material in the neodymium iron boron magnetic body that makes in 300～2500ppm scope.
Obtain in that the solution of the present invention is analysed in depth, the particle size of adding the performance raising amount of the neodymium-iron-boron magnetic material that the Graphene powder produces and selected NdFeB magnetic powder and Graphene powder is closely related.Therefore the present invention analyzes by the neodymium-iron-boron magnetic material performance that the NdFeB magnetic powder and the Graphene powder of a large amount of different-grain diameter sizes are prepared and optimizes, preferably choose NdFeB magnetic powder that particle diameter is 2～10um and thickness and be 3～5nm, diameter and be the graphene powder of 50～1000nm and produce neodymium-iron-boron magnetic material, make the magnetic property of NdFeB material farthest to be enhanced.
Further scheme is, NdFeB magnetic powder is to cast sheet by the Nd Fe B alloys of 0.2～10mm to become the elementary flour of particle diameter below 10mm through the hydrogen break process, elementary flour is ground through air-flow to obtain then; NdFeB magnetic powder and Graphene powder carry out mixing under inert gas shielding.With vertical orientated and preliminary compression moulding in the magnetic field of mixed powder more than 1.2T, and then through etc. static pressure handle and to be pressed into blank.Described sintering heat treatment is meant blank is placed 1000～1300 ℃ of sintering 1～4h in the vacuum drying oven sintering furnace; And then carry out one-level temper and second annealing processing, and wherein the temperature of one-level temper is 800～1000 ℃, time 1～4h, and the temperature that second annealing is handled is 400～600 ℃, time 1～4h.Wherein Nd Fe B alloys casting sheet can be by with various simple metal Nd, and Pr, Dy, Al, Ga, Co, Fe and alloy B-Fe, Nb-Fe etc. join by component design requirements and get raw material, cast at vacuum induction that melting obtains in the sheet stove.Further control by above process conditions makes that the performance of producing the neodymium-iron-boron magnetic material that obtains is excellent more.
The specific embodiment
Below come technical scheme of the present invention is done further explanation and explanation by specific embodiment, but should not be construed as qualification to protection domain of the present invention.
Embodiment 1
1, selecting model is that (its component consists of the 42SH magnetic material: Nd
27.8Fe
65.68B
1.02Dy
4.2Al
0.2.Co
1.0Cu
0.1) component design join and get raw material, then raw material is smelted into the casting sheet in vacuum induction casting sheet stove, the average thickness of casting sheet is 0.3-0.45mm;
2, the above-mentioned Nd-Fe-B alloy casting piece that obtains is positioned over carries out hydrogen decrepitation in the hydrogen crushing furnace and handle, obtain granularity at 10mm with interior elementary flour;
3, the elementary flour after the above-mentioned hydrogen fragmentation is milled to the NdFeB magnetic powder of particle diameter scope in 3 μ m-5 μ m through airflow milling technology; (thickness is that 3-5nm, diameter are that the mixed powder craft of 50～1000nm) warps mixes, and the carbon content in the control mixed powder is between 400-1000ppm to add the 0.03wt% graphene powder under nitrogen protection.
4, with mixed powder vertical orientated compression moulding in 1.8T magnetic field, be pressed into base through isostatic pressing process then;
5, above-mentioned blank is put into 1050 ℃ of sintering 2h of high vacuum sintering furnace, 900 ℃ of one-level temperatures, time 2h, 500 ℃ of second annealing temperature, time 3h makes the neodymium-iron-boron magnetic material that adds the Graphene powder.
Check experiment:
Do not add the Graphene powder in above-mentioned 3 steps, all the other operations are identical with embodiment, make the neodymium-iron-boron magnetic material that does not add graphene powder.
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out magnetism testing with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 1:
The magnetic property testing result of the sample that table 1 is produced for embodiment 1
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out mechanical property (compression strength) test with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 2:
The mechanical property testing result of the sample that table 2 is produced for embodiment 1
| Classification | Performance | Specification | State | Compression strength (N/mm 2） |
| Add Graphene | 42SH | 10*10*15 | Black-film | 850 |
| Do not add Graphene | 42SH | 10*10*15 | Black-film | 775 |
Embodiment 2
1, selecting model is that (its component consists of Nd to the N48 magnetic material
31.8Fe
65.58B
1.02Co
1.0Cu
0.1Al
0.3Ga
0.2) component design join and get raw material, then it is smelted into the casting sheet in vacuum induction casting sheet stove, the average thickness of casting sheet is 0.2-0.45mm;
2, the above-mentioned Nd-Fe-B alloy casting piece that obtains is positioned over carries out hydrogen decrepitation in the hydrogen crushing furnace and handle, obtain granularity at 10mm with interior elementary flour;
3, the elementary flour that obtains after the above-mentioned hydrogen fragmentation is milled to the NdFeB magnetic powder of particle diameter scope in 3 μ m-5 μ m through airflow milling technology, (thickness is that 3-5nm, diameter are that the mixed powder craft of 50～1000nm) warps mixes, and the carbon content in the control mixed powder is between 800-1200ppm to add the 0.06wt% graphene powder under nitrogen protection;
4, with mixed powder vertical orientated compression moulding in 1.2T magnetic field, be pressed into base through isostatic pressing process then;
5, above-mentioned blank is put into 1000 ℃ of sintering 2h of high vacuum sintering furnace, 900 ℃ of one-level temperatures, time 2h, 500 ℃ of second annealing temperature, time 3h makes the neodymium-iron-boron magnetic material that adds the Graphene powder.
Check experiment:
Do not add the Graphene powder in above-mentioned 3 steps, all the other operations are identical with embodiment, make the neodymium-iron-boron magnetic material that does not add graphene powder.
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out magnetism testing with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 3:
The magnetic property testing result of the sample that table 3 is produced for embodiment 2
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out mechanical property (compression strength) test with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 4:
The mechanical property testing result of the sample that table 4 is produced for embodiment 2
| Classification | Performance | Specification | State | Compression strength (N/mm 2） |
| Add Graphene | N48 | 10*10*15 | Black-film | 885 |
| Do not add Graphene | N48 | 10*10*15 | Black-film | 786 |
Embodiment 3
1, selecting model is that (its component consists of the 33UH magnetic material: Nd
26Fe
64.78B
1.02Dy
6.0Co
1.5Cu
0.1Al
0.6) component design join and get raw material, then raw material is smelted into the casting sheet in vacuum induction casting sheet stove, the average thickness of casting sheet is 0.3-0.45mm;
2, above-mentioned Nd-Fe-B alloy casting piece is positioned over carries out hydrogen decrepitation in the hydrogen crushing furnace and handle, the granularity of the broken powder of the hydrogen that obtains is controlled at 10mm with interior elementary flour;
3, the elementary flour after the above-mentioned hydrogen fragmentation is worn into the NdFeB magnetic powder of particle diameter scope in 3 μ m-5 μ m through airflow milling technology; adding 0.08wt% graphene powder under nitrogen protection (thickness is that 3-5nm, diameter are that the mixed powder craft of 50～1000nm) warps mixes, and the carbon content in the control mixed powder is 900-1400ppm:
4, with mixed powder vertical orientated compression moulding in 1.8T magnetic field, be pressed into base through isostatic pressing process then;
5, above-mentioned blank is put into 1050 ℃ of sintering 4h of high vacuum sintering furnace, 800 ℃ of one-level temperatures, time 4h, 500 ℃ of second annealing temperature, time 4h makes the neodymium-iron-boron magnetic material that adds the Graphene powder.
Check experiment:
Do not add the Graphene powder in above-mentioned 3 steps, all the other operations are identical with embodiment, make the neodymium-iron-boron magnetic material that does not add graphene powder.
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out magnetism testing with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 5:
The magnetic property testing result of the sample that table 5 is produced for embodiment 3
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out mechanical property (compression strength) test with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 6:
The mechanical property testing result of the sample that table 6 is produced for embodiment 3
| Classification | Performance | Specification | State | Compression strength (N/mm 2） |
| Add Graphene | 33UH | 10*10*15 | Black-film | 901 |
| Do not add Graphene | 33UH | 10*10*15 | Black-film | 788 |
Embodiment 4
1, be that (its component consists of the 48M magnetic material: Nd according to model
30.5Fe
65.4B
1.0Dy
1.8Co
0.8Cu
0.1Zr
0.2Ga
0.2) component design join and get raw material, then raw material is smelted into the casting sheet in vacuum induction casting sheet stove, the average thickness of casting sheet is 0.3-0.45mm;
2, above-mentioned Nd-Fe-B alloy casting piece is positioned over carries out hydrogen decrepitation in the hydrogen crushing furnace and handle, the granularity of the broken powder of the hydrogen that obtains is controlled at 10mm with interior elementary flour;
3, the elementary flour after the above-mentioned hydrogen fragmentation is worn into the NdFeB magnetic powder of particle diameter scope in 3 μ m-5 μ m through airflow milling technology; adding 0.10wt% graphene powder under nitrogen protection (thickness is that 3-5nm, diameter are that the mixed powder craft of 50～1000nm) warps mixes, and the carbon content in the control mixed powder is between 1200-1600ppm:
4, with mixed powder vertical orientated compression moulding in 1.8T magnetic field, be pressed into base through isostatic pressing process then;
5, above-mentioned blank is put into 1300 ℃ of sintering 1h of high vacuum sintering furnace, 1000 ℃ of one-level temperatures, time 1h, 500 ℃ of second annealing temperature, time 3h makes the neodymium-iron-boron magnetic material that adds the Graphene powder.
Check experiment:
Do not add the Graphene powder in above-mentioned 3 steps, all the other operations are identical with embodiment, make the neodymium-iron-boron magnetic material that does not add graphene powder.
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out magnetism testing with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 7:
The magnetic property testing result of the sample that table 7 is produced for embodiment 4
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out mechanical property (compression strength) test with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 8:
The mechanical property testing result of the sample that table 8 is produced for embodiment 4
| Classification | Performance | Specification | State | Compression strength (N/mm 2） |
| Add Graphene | 48M | 10*10*15 | Black-film | 910 |
| Do not add Graphene | 48M | 10*10*15 | Black-film | 776 |
Embodiment 5
1, (its component consists of: Nd for the 40H magnetic material according to model
29.6Fe
66.28B
1.02Dy
2.0Co
0.6Cu
0.1Al
0.4) component design join and get raw material, then raw material is smelted into the casting sheet in vacuum induction casting sheet stove, the average thickness of casting sheet is 0.3-0.45mm;
2, above-mentioned Nd-Fe-B alloy casting piece is positioned over carries out hydrogen decrepitation in the hydrogen crushing furnace and handle, the granularity of the broken powder of the hydrogen that obtains is controlled at 10mm with interior elementary flour;
3, the elementary flour after the above-mentioned hydrogen fragmentation is worn into the NdFeB magnetic powder of particle diameter scope in 3 μ m-5 μ m through airflow milling technology; adding 0.15wt% graphene powder under nitrogen protection (thickness is that 3-5nm, diameter are that the mixed powder craft of 50～1000nm) warps mixes, and the carbon content in the control mixed powder is between 1700-2000ppm:
4, with mixed powder vertical orientated compression moulding in 1.8T magnetic field, be pressed into base through isostatic pressing process then;
5, above-mentioned blank is put into 1050 ℃ of sintering 2h of high vacuum sintering furnace, 900 ℃ of one-level temperatures, time 2h, 500 ℃ of second annealing temperature, time 1h makes the neodymium-iron-boron magnetic material that adds the Graphene powder.
Check experiment:
Do not add the Graphene powder in above-mentioned 3 steps, all the other operations are identical with embodiment, make the neodymium-iron-boron magnetic material that does not add graphene powder.
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out magnetism testing with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 9:
The magnetic property testing result of the sample that table 9 is produced for embodiment 5
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out mechanical property (compression strength) test with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 10:
The mechanical property testing result of the sample that table 10 is produced for embodiment 5
| Classification | Performance | Specification | State | Compression strength (N/mm 2） |
| Add Graphene | 40H | 10*10*15 | Black-film | 922 |
| Do not add Graphene | 40H | 10*10*15 | Black-film | 778 |
Embodiment 6
1, be that (its component consists of the N52 magnetic material: Nd according to model
30.0Fe
66.98B
1.02Dy
0.4Co
0.9Cu
0.1Al
0.1) component design join and get raw material, then raw material is smelted into the casting sheet in vacuum induction casting sheet stove, the average thickness of casting sheet is 0.45-0.85mm;
2, above-mentioned Nd-Fe-B alloy casting piece is positioned over carries out hydrogen decrepitation in the hydrogen crushing furnace and handle, the granularity of the broken powder of the hydrogen that obtains is controlled at 10mm with interior elementary flour;
3, the elementary flour after the above-mentioned hydrogen fragmentation is worn into the NdFeB magnetic powder of particle diameter scope in 3 μ m-5 μ m through airflow milling technology; adding 0.20wt% graphene powder under nitrogen protection (thickness is that 3-5nm, diameter are that the mixed powder craft of 50～1000nm) warps mixes, and the carbon content in the control mixed powder is between 2100-2500ppm:
4, with mixed powder vertical orientated compression moulding in 1.8T magnetic field, be pressed into base through isostatic pressing process then;
5, above-mentioned blank is put into 1050 ℃ of sintering 2h of high vacuum sintering furnace, 900 ℃ of one-level temperatures, time 2h, 500 ℃ of second annealing temperature, time 3h makes the neodymium-iron-boron magnetic material that adds the Graphene powder.
Check experiment:
Do not add the Graphene powder in above-mentioned 3 steps, all the other operations are identical with embodiment, make the neodymium-iron-boron magnetic material that does not add graphene powder.
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out magnetism testing with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 11:
The magnetic property testing result of the sample that table 11 is produced for embodiment 6
Neodymium-iron-boron magnetic material sample to the interpolation Graphene powder that obtains behind the sintering carries out mechanical property (compression strength) test with the sample of magnetic material of not adding the Graphene powder, shown in the table with test results 12:
The mechanical property testing result of the sample that table 12 is produced for embodiment 6
| Classification | Performance | Specification | State | Compression strength (N/mm 2） |
| Add Graphene | N52 | 10*10*15 | Black-film | 930 |
| Do not add Graphene | N52 | 10*10*15 | Black-film | 775 |
For saving space, the adding proportion and the part technology of only part Graphene powder being mixed illustrates here.Above embodiment shows, technologies such as die mould, sintering behind the graphene powder of interpolation trace in through the magnetic after the airflow milling, mechanical property of gained sintered Nd-Fe-B magnetic material (compression strength) and magnetic property have all obtained corresponding raising, this makes the processability of neodymium-iron-boron magnetic material be significantly improved, and product in use keeps the ability of permanent magnetism stronger, and range of application is more extensive.
Claims (7)
1. method for preparing NdFeB material, its operation is as follows: NdFeB magnetic powder and Graphene powder mixing are configured to mixed powder, again mixed powder is orientated and is pressed into blank in magnetic field, then blank is carried out sintering heat treatment and can produce and obtain NdFeB material; The content of Graphene powder is 0.03～0.20wt% in the mixed powder; The composition of described NdFeB magnetic powder is R
wQ
xM
yN
z, wherein R is one or more in Pr, Nd, Dy, Tb, Ho, the Gd element, and Q is one or both in Fe, the Co element, and M is the B element, and N is one or more in Al, Nb, Zr, Cu, Ga, Mo, W, the V element; 29≤w≤33,60≤x≤69,0.98≤y≤1.2,0≤z≤3, w+x+y+z=100.
2. the method for preparing NdFeB material as claimed in claim 1 is characterized in that: carbon content is 300～2500ppm in the neodymium iron boron magnetic body that makes.
3. the method for preparing NdFeB material as claimed in claim 1 is characterized in that: the particle diameter of described NdFeB magnetic powder is 2～10um; The thickness of described graphene powder is 3～5nm, and diameter is 50～1000nm.
4. the method for preparing NdFeB material as claimed in claim 1 is characterized in that: described sintering heat treatment is meant blank is placed 1000～1300 ℃ of sintering 1～4h in the vacuum drying oven sintering furnace; And then carry out one-level temper and second annealing processing, and wherein the temperature of one-level temper is 800～1000 ℃, time 1～4h, and the temperature that second annealing is handled is 400～600 ℃, time 1～4h.
5. the method for preparing NdFeB material as claimed in claim 1 is characterized in that: NdFeB magnetic powder and Graphene powder carry out mixing under inert gas shielding.
6. the method for preparing NdFeB material as claimed in claim 1 is characterized in that: be will be in the magnetic field of mixed powder more than 1.2T orientation and preliminary compression moulding, and then through waiting static pressure processing to be pressed into blank.
7. the method for preparing NdFeB material as claimed in claim 1, it is characterized in that: NdFeB magnetic powder is to be that the Nd Fe B alloys casting sheet of 0.2～10mm becomes the elementary flour of particle diameter below 10mm through the hydrogen break process by thickness, elementary flour is ground through air-flow to obtain then.
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