CN101615461A - Nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet and preparation method thereof - Google Patents

Nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet and preparation method thereof Download PDF

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CN101615461A
CN101615461A CN200910098783A CN200910098783A CN101615461A CN 101615461 A CN101615461 A CN 101615461A CN 200910098783 A CN200910098783 A CN 200910098783A CN 200910098783 A CN200910098783 A CN 200910098783A CN 101615461 A CN101615461 A CN 101615461A
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严密
崔熙贵
马天宇
罗伟
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Zhejiang University ZJU
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Abstract

The invention discloses a kind of preparation method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet.The steps include: 1) main-phase alloy and crystal-boundary phase alloy prepare respectively, and main-phase alloy adopts casting technique or rapid hardening belt-rejecting technology to make ingot casting or rapid hardening strip, and crystal-boundary phase alloy adopts rapid quenching technique to make rapid tempering belt; 2) with the main-phase alloy and the crystal-boundary phase alloy powder process respectively that prepare; 3) nanometer Zn powder is evenly mixed with the crystal-boundary phase alloy powder, make it be dispersed in the crystal-boundary phase alloy powder surface; 4) with the crystal-boundary phase alloy powder of nanometer Zn modification with after main-phase alloy powder is evenly mixed, the orientation die mould is made green compact in magnetic field; 5) final magnet is made in green compact sintering and tempering in high vacuum sintering furnace.The Sintered NdFeB magnet performance height that the present invention makes, good corrosion resistance, and also technology is simple, easy to operate, is suitable for large-scale mass production.

Description

Nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet and preparation method thereof
Technical field
The present invention relates to a kind of preparation method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet.
Background technology
Sintered NdFeB magnet is the rare earth permanent-magnetic material of releasing early 1980s of new generation, it has excellent comprehensive magnetic property, high cost performance and easy advantage such as processing, now has been widely used in fields such as computer, motor, wind-driven generator, electric automobile, instrument and meter, high-fidelity loudspeaker, NMR imaging instrument and space flight and aviation omniselector.Because its high magnetic energy product, therefore suitablely especially be applied to require in miniaturization, lightweight, the integrated various regeneration products.
Sintered NdFeB magnet is with Nd 2Fe 14The B compound is a matrix, and its magnetic property derives from Nd 2Fe 14The intrinsic magnetic parameter of B compound is as H A, J s, T cDeng.The magnetic property of Sintered NdFeB magnet is used remanent magnetism B usually r, coercive force H Cj, magnetic energy product (BH) MaxCharacterize B rLimiting value be J s, (BH) MaxLimiting value be 1/4J s 2, H CjLimiting value be magnetocrystalline anisotropy field H A, it depends on the magnetocrystalline anisotropy constant K of material 1And K 2The raising of magnetic property all is researcher's a research emphasis all the time, and through effort for many years, the maximum magnetic energy product of the magnet of prepared in laboratory has reached 474kJ/m 3, near 93% of theoretical value.Yet actual coercive force only is the 1/3-1/30 of its theoretical value, thereby also has great potentialities and can dig in the coercitive raising of Sintered NdFeB magnet.Along with the progressively raising of magnetic property, the shortcoming of Sintered NdFeB magnet corrosion-resistant day by day is exaggerated, and has limited the further expansion of its range of application.
Sintered NdFeB magnet is a polycrystalline complex phase permanent material, mainly by principal phase Nd 2Fe 14B, boron-rich phase and rich neodymium phase composition.Rich neodymium mainly evenly distributes along the principal phase crystal boundary mutually, and boron-rich phase mainly is present in the crystal boundary with graininess.Because the electrode potential of rich neodymium phase is far below principal phase Nd 2Fe 14Therefore B can constitute corrosion galvanic cell between them in corrosive medium, the negative rich neodymium of current potential becomes anode in primary cell, preferentially corrode, and the motive power of its corrosion is principal phase Nd 2Fe 14B and crystal boundary mutually, the electrochemistry potential difference that especially rich neodymium is alternate.Because the negligible amounts of rich neodymium phase in the Sintered NdFeB magnet, therefore, the local corrosion battery has the characteristics of the big negative electrode of primary anode, born very big corrosion electric current density mutually as a small amount of rich neodymium of anode, quickened the intercrystalline corrosion of rich neodymium phase, as seen, the corrosion of Sintered NdFeB magnet is typical intercrystalline corrosion, reduces principal phase Nd 2Fe 14The electrochemistry potential difference that B is alternate with rich neodymium is to improve the effective means of its intrinsic decay resistance.
The pairing gold process is as the term suggests certainly exist two kinds of alloys, and in sintered nd-fe-b magnet, these two kinds of alloys are respectively nearly Nd 2Fe 14The main-phase alloy of the positive composition ratio of B and the crystal-boundary phase alloy of rich Nd.With independent melting and the powder process respectively of these two kinds of alloys, main-phase alloy is usually by ingot casting or the preparation of rapid hardening belt-rejecting technology, and auxilliary phase alloy is usually with quick quenching technique preparation, powder process respectively then, at last both are mixed according to a certain percentage, carry out magnetic field orientating moulding and sintering again and make magnet.Utilize the pairing gold process to prepare Sintered NdFeB magnet and can be easily and effectively carry out modification mutually, thereby improve its electrode potential, reduce itself and the electrochemistry potential difference of principal phase, the decay resistance of raising magnet the rich neodymium of crystal boundary.In addition, the improvement of crystal boundary phase physicochemical property helps microstructural optimization, can improve the magnetic property of magnet simultaneously.Therefore, we can utilize this principle to improve the combination property of sintered Nd-Fe-B permanent magnet.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet is provided.
The preparation method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet comprises the steps:
1) main-phase alloy adopts casting technique or rapid hardening belt-rejecting technology to make ingot casting or rapid hardening strip, and crystal-boundary phase alloy adopts rapid quenching technique to make rapid tempering belt; Carry out coarse crushing by Mechanical Crushing or hydrogen explosion are broken respectively then, coarse crushing is after ball milling or airflow milling fine grinding, and making average particulate diameter is the main-phase alloy powder of 2-10 μ m and the crystal-boundary phase alloy powder of 1-8 μ m;
2) adding percentage by weight in the crystal-boundary phase alloy powder is the nanometer Zn powder of 1%-20% and the antioxidant of 1%-10%, obtains the crystal-boundary phase alloy powder of nanometer Zn modification after evenly mixing;
3) be that the crystal-boundary phase alloy powder of the nanometer Zn modification of 1-20% adds in the main-phase alloy powder with percentage by weight, adding percentage by weight is the gasoline of 0.5%-5%, evenly is mixed and made into mixed-powder then in batch mixer;
4) mixed-powder is orientated die mould and makes green compact in the magnetic field of 1.2-2.0T;
5) with green compact at 1050-1125 ℃ of following vacuum-sintering 2-4h, through 850-950 ℃ of one-level tempering 2-4h and 500-650 ℃ of second annealing 2-4h, make magnet again.
The atomic percent of described main-phase alloy composition is Nd xFe 100-x-y-zB yM z, 11≤x≤16,5.5≤y≤7,0.1≤z≤10 wherein, M is one or more in Pr, Dy, Tb, Co, Al, Cu, Ga, Nb, Zr, Ti, the Mo element.
The atomic percent of described crystal-boundary phase alloy composition is Nd aFe 100-a-b-cB bR c, 12≤a≤30,5≤b≤7,0.1≤c≤20 wherein, R is one or more in Pr, Dy, Tb, Co, Al, Cu, Ga, Si, Nb, Zr, Ti, Mo, W, the V element.
The average particulate diameter of described nanometer Zn powder is 2-80nm.
The magnet that the present invention makes is than having higher magnetic property and better decay resistance without the nanometer Zn crystal boundary modified magnet that makes, technical process is simple, and is easy to operate, is suitable for mass production.
Embodiment
The present invention adopts the pairing gold process to prepare Sintered NdFeB magnet, main-phase alloy and crystal-boundary phase alloy prepare respectively, by mixing of nanometer Zn and crystal-boundary phase alloy powder, nanometer Zn is dispersed in crystal boundary phase powder particle surface, to decay resistance and the magnetic property of modified grain boundary phase with the raising Sintered NdFeB magnet.Crystal boundary through the nanometer Zn modification has higher electrochemical bit mutually, has reduced the electrochemistry potential difference between itself and principal phase, thereby has effectively improved the decay resistance of magnet.In addition, it is beneficial to and is distributed in principal phase Nd more equably 2Fe 14The B grain surface plays the effect of degaussing exchange coupling, is beneficial to the sintering densification of magnet simultaneously, has improved the density of magnet, thereby has improved the comprehensive magnetic property of magnet.
The preparation method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet comprises the steps:
1) main-phase alloy adopts casting technique or rapid hardening belt-rejecting technology to make ingot casting or rapid hardening strip, and crystal-boundary phase alloy adopts rapid quenching technique to make rapid tempering belt; Carry out coarse crushing by Mechanical Crushing or hydrogen explosion are broken respectively then, coarse crushing is after ball milling or airflow milling fine grinding, and making average particulate diameter is the main-phase alloy powder of 2-10 μ m and the crystal-boundary phase alloy powder of 1-8 μ m;
2) adding percentage by weight in the crystal-boundary phase alloy powder is the nanometer Zn powder of 1%-20% and the antioxidant of 1%-10%, obtains the crystal-boundary phase alloy powder of nanometer Zn modification after evenly mixing;
3) be that the crystal-boundary phase alloy powder of the nanometer Zn modification of 1-20% adds in the main-phase alloy powder with percentage by weight, adding percentage by weight is the gasoline of 0.5%-5%, evenly is mixed and made into mixed-powder then in batch mixer;
4) mixed-powder is orientated die mould and makes green compact in the magnetic field of 1.2-2.0T;
5) with green compact at 1050-1125 ℃ of following vacuum-sintering 2-4h, through 850-950 ℃ of one-level tempering 2-4h and 500-650 ℃ of second annealing 2-4h, make magnet again.
The particular content of casting technique of the present invention, rapid hardening belt-rejecting technology, rapid quenching technique, the broken technology of hydrogen explosion is seen Zhou Shouzeng, Dong Qingfei " superpower permanet magnetic body---rare-earth system permanent magnetic material " Beijing respectively, metallurgical industry publishing house, 2004.2 second edition, p159-164, p498-504, p326-332, p508-511, p169-172.
Embodiment 1:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.Main-phase alloy adopts the preparation of rapid hardening belt-rejecting technology, and copper roller linear resonance surface velocity is 1.6m/s, and composition is Nd 12.2Dy 0.2Fe BalAl 0.4Zr 0.1B 5.8(at%), crystal-boundary phase alloy adopts the rapid quenching technique preparation, and fast quenching speed is 23m/s, and composition is Nd 20Dy 2Fe BalGa 0.5Nb 0.5B 6.5(at%);
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Undertaken slightly breaking by jaw crusher, broken in being undertaken by middle disintegrating machine, under nitrogen protection, make the powder that average particulate diameter is 3.6 μ m and 2.8 μ m respectively then by airflow milling;
3) adding percentage by weight is 5%, average particulate diameter is 20nm nanometer Zn powder and weight ratio in the crystal-boundary phase alloy powder is 4% antioxidant, evenly mixes in batch mixer;
4) the crystal-boundary phase alloy powder with the nanometer Zn modification adds in the main-phase alloy powder, and its percentage by weight is 1%, and to add percentage by weight be 0.5% gasoline, evenly is mixed and made into mixed-powder then in batch mixer;
5) mixed-powder is orientated die mould in the magnetic field of 2.0T and makes green compact;
6) with green compact at 1065 ℃ of following vacuum-sintering 3h, through 880 one-level tempering 2h and 510 ℃ of second annealing 3h, make final magnet again;
7) preparation of employing same process is added the crystal-boundary phase alloy of weight ratio 1% but is not added the magnet of nanometer Zn.
(5-10psig, 100h) has tested sample (1 * 1 * 1cm) corrosion resistance, result such as table one by 110-115 ℃ to adopt autoclave test.
Table one adds and the decay resistance that does not add the nanometer Zn magnet
Classification Quality (mg) before the test Test back quality (mg) Mass loss (mg/cm 2)
Do not add nanometer Zn ??7520 ??7392 ??128
Add nanometer Zn ??7550 ??7518 ??32
Therefrom as can be seen, after the interpolation nanometer Zn, the corrosion resistance of Sintered NdFeB magnet is better than the magnet that does not add nanometer Zn, therefore, can prepare the Sintered NdFeB magnet of highly corrosion resistant by the modification of nanometer Zn crystal boundary phase.
Embodiment 2:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.Main-phase alloy adopts the casting technique preparation, and composition is Nd 13.8Fe BalB 5.95(at%), crystal-boundary phase alloy adopts the rapid quenching technique preparation, and fast quenching speed is 16m/s, and composition is Nd 17Dy 3Tb 0.5Fe BalGa 0.1Cu 0.4B 6.2(at%);
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Carry out coarse crushing by the quick-fried method of hydrogen, under nitrogen protection, make the powder that average particulate diameter is 4.2 μ m and 3.5 μ m respectively then by airflow milling;
3) adding percentage by weight is 20%, average particulate diameter is 40nm nanometer Zn powder and weight ratio in the crystal-boundary phase alloy powder is 2% antioxidant, evenly mixes in batch mixer;
4) the crystal-boundary phase alloy powder with the nanometer Zn modification adds in the main-phase alloy powder, and its percentage by weight is 10%, and to add percentage by weight be 2% gasoline, evenly is mixed and made into mixed-powder then in batch mixer;
5) mixed-powder is orientated die mould in the magnetic field of 1.8T and makes green compact;
6) with green compact at 1080 ℃ of following vacuum-sintering 2.5h, through 890 ℃ of one-level tempering 2h and 530 ℃ of second annealing 2.5h, make final magnet again;
7) preparation of employing same process is added the crystal-boundary phase alloy of weight ratio 10% but is not added the magnet of nanometer Zn.
(5-10psig, 100h) has tested sample (1 * 1 * 1cm) corrosion resistance, result such as table two by 110-115 ℃ to adopt autoclave test.
Table two adds and the decay resistance that does not add the nanometer Zn magnet
Classification Quality (mg) before the test Test back quality (mg) Mass loss (mg/cm 2)
Do not add nanometer Zn ??7480 ??7294 ??186
Add nanometer Zn ??7520 ??7479 ??41
Therefrom as can be seen, after the interpolation nanometer Zn, the corrosion resistance of Sintered NdFeB magnet is better than the magnet that does not add nanometer Zn, therefore, can prepare the Sintered NdFeB magnet of highly corrosion resistant by the modification of nanometer Zn crystal boundary phase.
Embodiment 3:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.Main-phase alloy adopts the preparation of rapid hardening belt-rejecting technology, and copper roller linear resonance surface velocity is 1.2m/s, and composition is Nd 11Pr 5Dy 0.5Fe BalB 6(at%), crystal-boundary phase alloy adopts the rapid quenching technique preparation, and fast quenching speed 20m/s, composition are Nd 12Dy 3.49Fe BalCo 10.1Cu 2.8B 6.7(at%);
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Undertaken slightly breaking by jaw crusher, broken in being undertaken by middle disintegrating machine, under nitrogen protection, make the powder that average particulate diameter is 3.0 μ m and 2.2 μ m then by the airflow milling proportion by subtraction;
3) adding percentage by weight is 5%, average particulate diameter is 10nm nanometer Zn powder and weight ratio in the crystal-boundary phase alloy powder is 1% antioxidant, evenly mixes in batch mixer;
4) the crystal-boundary phase alloy powder with the nanometer Zn modification adds in the main-phase alloy powder, and its percentage by weight is 15%, and to add percentage by weight be 5% gasoline, evenly is mixed and made into mixed-powder then in batch mixer;
5) mixed-powder is orientated die mould in the magnetic field of 1.6T and makes green compact;
6) with green compact at 1095 ℃ of following vacuum-sintering 2h, through 900 ℃ of one-level tempering 2h and 560 ℃ of second annealing 2h, make final magnet again;
7) preparation of employing same process is added the crystal-boundary phase alloy of weight ratio 15% but is not added the magnet of nanometer Zn.
(5-10psig, 100h) has tested sample (1 * 1 * 1cm) corrosion resistance, result such as table three by 110-115 ℃ to adopt autoclave test.
Table three adds and the decay resistance that does not add the nanometer Zn magnet
Classification Quality (mg) before the test Test back quality (mg) Mass loss (mg/cm 2)
Do not add nanometer Zn ??7490 ??7337 ??153
Add nanometer Zn ??7510 ??7473 ??37
Therefrom as can be seen, after the interpolation nanometer Zn, the corrosion resistance of Sintered NdFeB magnet is better than the magnet that does not add nanometer Zn, therefore, can prepare the Sintered NdFeB magnet of highly corrosion resistant by the modification of nanometer Zn crystal boundary phase.
Embodiment 4:
1) main-phase alloy and crystal-boundary phase alloy are prepared respectively.The main-phase alloy composition is Nd 14.8Dy 1Fe BalNb 0.15B 6(at%), adopt the preparation of rapid hardening belt-rejecting technology, copper roller linear resonance surface velocity is 2m/s,, the crystal-boundary phase alloy composition is Nd 25Pr 5Dy 2Fe BalCo 5Cu 1.2Zr 0.5Al 2.2B 7(at%), adopt the rapid quenching technique preparation, fast quenching speed is 18m/s;
2) with main-phase alloy and crystal-boundary phase alloy powder process respectively.Carry out coarse crushing by the quick-fried method of hydrogen, under the benzinum protection, make the powder that average particulate diameter is 6 μ m and 4.3 μ m respectively then by ball milling;
3) adding percentage by weight is 1%, average particulate diameter is 20nm nanometer Zn powder and weight ratio in the crystal-boundary phase alloy powder is 10% antioxidant, evenly mixes in batch mixer;
4) the crystal-boundary phase alloy powder with the nanometer Zn modification adds in the main-phase alloy powder, and its percentage by weight is 20%, and to add percentage by weight be 3% gasoline, evenly is mixed and made into mixed-powder then in batch mixer;
5) mixed-powder is orientated die mould in the magnetic field of 1.2T and makes green compact;
6) with green compact at 1125 ℃ of following vacuum-sintering 2h, through 920 ℃ of one-level tempering 2h and 610 ℃ of second annealing 4h, make final magnet again;
7) preparation of employing same process is added the crystal-boundary phase alloy of weight ratio 20% but is not added the magnet of nanometer Zn.
(5-10psig, 100h) has tested sample (1 * 1 * 1cm) corrosion resistance, result such as table four by 110-115 ℃ to adopt autoclave test.
Table four adds and the decay resistance that does not add the nanometer Zn magnet
Classification Quality (mg) before the test Test back quality (mg) Mass loss (mg/cm 2)
Do not add nanometer Zn ??7550 ??7453 ??97
Add nanometer Zn ??7580 ??7558 ??22
Therefrom as can be seen, after the interpolation nanometer Zn, the corrosion resistance of Sintered NdFeB magnet is better than the magnet that does not add nanometer Zn, therefore, can prepare the Sintered NdFeB magnet of highly corrosion resistant by the modification of nanometer Zn crystal boundary phase.

Claims (4)

1. the preparation method of a nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet is characterized in that comprising the steps:
1) main-phase alloy adopts casting technique or rapid hardening belt-rejecting technology to make ingot casting or rapid hardening strip, and crystal-boundary phase alloy adopts rapid quenching technique to make rapid tempering belt; Carry out coarse crushing by Mechanical Crushing or hydrogen explosion are broken respectively then, coarse crushing is after ball milling or airflow milling fine grinding, and making average particulate diameter is the main-phase alloy powder of 2-10 μ m and the crystal-boundary phase alloy powder of 1-8 μ m;
2) adding percentage by weight in the crystal-boundary phase alloy powder is the nanometer Zn powder of 1%-20% and the antioxidant of 1%-10%, obtains the crystal-boundary phase alloy powder of nanometer Zn modification after evenly mixing;
3) be that the crystal-boundary phase alloy powder of the nanometer Zn modification of 1-20% adds in the main-phase alloy powder with percentage by weight, adding percentage by weight is the gasoline of 0.5%-5%, evenly is mixed and made into mixed-powder then in batch mixer;
4) mixed-powder is orientated die mould and makes green compact in the magnetic field of 1.2-2.0T;
5) with green compact at 1050-1125 ℃ of following vacuum-sintering 2-4h, through 850-950 ℃ of one-level tempering 2-4h and 500-650 ℃ of second annealing 2-4h, make magnet again.
2. the preparation method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet according to claim 1, the atomic percent that it is characterized in that described main-phase alloy composition is Nd xFe 100-x-y-zB yM z, 11≤x≤16,5.5≤y≤7,0.1≤z≤10 wherein, M is one or more in Pr, Dy, Tb, Co, Al, Cu, Ga, Nb, Zr, Ti, the Mo element.
3. the preparation method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet according to claim 1, the atomic percent that it is characterized in that described crystal-boundary phase alloy composition is Nd aFe 100-a-b-cB bR c, 12≤a≤30,5≤b≤7,0.1≤c≤20 wherein, R is one or more in Pr, Dy, Tb, Co, Al, Cu, Ga, Si, Nb, Zr, Ti, Mo, W, the V element.
4. the Preparation Method of nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet system according to claim 1, the average particulate diameter that it is characterized in that described nanometer Zn powder is 2-80nm.
CN200910098783A 2009-05-14 2009-05-14 Nanometer Zn crystal boundary modified high-corrosion resistance Sintered NdFeB magnet and preparation method thereof Pending CN101615461A (en)

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CN103680919B (en) * 2013-12-13 2016-09-07 北京科技大学 A kind of preparation method of the high anti-corrosion sintered Nd-Fe-B permanent magnet of tough height of high-coercive force
CN103680919A (en) * 2013-12-13 2014-03-26 北京科技大学 Method for preparing high-coercivity, high-toughness and high-corrosion-resistance sintered Nd-Fe-B permanent magnet
CN103928204A (en) * 2014-04-10 2014-07-16 重庆科技学院 Low-rare earth content anisotropy nanocrystalline NdFeB compact magnet and preparation method thereof
WO2016086398A1 (en) * 2014-12-04 2016-06-09 浙江大学 Method for preparing high-coercivity sinterednd-fe-b and product obtained thereby
CN106158212A (en) * 2014-12-11 2016-11-23 乔俊擎 A kind of sintered Nd-Fe-B permanent magnetic material and preparation method thereof
CN106158212B (en) * 2014-12-11 2018-07-03 安徽省瀚海新材料股份有限公司 A kind of sintered Nd-Fe-B permanent magnetic material and preparation method thereof
CN105118649A (en) * 2015-06-18 2015-12-02 浙江东阳东磁稀土有限公司 Method for improving grain boundary phase of neodymium iron boron
CN107689279A (en) * 2017-09-13 2018-02-13 内蒙古科技大学 One kind improves the coercitive method of sintered NdFeB built-up magnet

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