CN115385676A - Method for preparing medium-high grade permanent magnetic ferrite by using iron ore concentrate powder as raw material - Google Patents
Method for preparing medium-high grade permanent magnetic ferrite by using iron ore concentrate powder as raw material Download PDFInfo
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- CN115385676A CN115385676A CN202211042068.7A CN202211042068A CN115385676A CN 115385676 A CN115385676 A CN 115385676A CN 202211042068 A CN202211042068 A CN 202211042068A CN 115385676 A CN115385676 A CN 115385676A
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- magnetic ferrite
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- 239000000843 powder Substances 0.000 title claims abstract description 199
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 90
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 61
- 239000012141 concentrate Substances 0.000 title claims abstract description 55
- 239000002994 raw material Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 114
- 238000005245 sintering Methods 0.000 claims abstract description 103
- 239000002002 slurry Substances 0.000 claims abstract description 45
- 238000001914 filtration Methods 0.000 claims abstract description 29
- 230000005291 magnetic effect Effects 0.000 claims abstract description 25
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 239000000654 additive Substances 0.000 claims abstract description 17
- 230000000996 additive effect Effects 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 15
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 13
- 239000011812 mixed powder Substances 0.000 claims description 13
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 10
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 10
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 239000004615 ingredient Substances 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004227 calcium gluconate Substances 0.000 claims description 3
- 229960004494 calcium gluconate Drugs 0.000 claims description 3
- 235000013927 calcium gluconate Nutrition 0.000 claims description 3
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 238000002485 combustion reaction Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 230000005389 magnetism Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 230000008569 process Effects 0.000 description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 230000005347 demagnetization Effects 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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Abstract
The invention relates to a method for preparing medium-high grade permanent magnetic ferrite by taking iron concentrate powder as a raw material, wherein the raw material of element Fe in the permanent magnetic ferrite adopts the iron concentrate powder, a sintering aid A and a sintering aid B are added when first slurry is prepared, wet material obtained by filtering the first slurry is presintered to form permanent magnetic ferrite presintering material, then the presintering material is crushed, a surfactant and a secondary additive are added to form second slurry by wet ball milling, wet material obtained by filtering the second slurry is prepared into green body to be sintered to obtain high magnetic performance permanent magnetic ferrite material, and the residual magnetism Br of the high magnetic performance permanent magnetic ferrite material is detected as follows: 420-430mT, coercive force HCB:285-310KA/m, intrinsic coercivity Hcj:340-370KA/m, maximum magnetic energy product BH (max) ：33‑34KJ/m 3 . The method breaks through the restriction of the raw materials on the preparation of middle-high grade permanent magnetic ferrite materials, and has the advantages ofIs beneficial to enlarging the production scale of the middle and high grade permanent magnetic ferrite material and reducing the cost.
Description
Technical Field
The invention belongs to the field of permanent magnetic ferrite preparation, and particularly relates to a preparation method of a medium-high grade permanent magnetic ferrite.
Background
The ferrite permanent magnetic material has the advantages of stable performance and low price, and has a large proportion in the market all the time. With the integration miniaturization of electronic devices, ferrite permanent magnetic materials are required to have higher magnetic properties, and high-performance high-grade permanent magnetic ferrites used in the current market are all prepared by taking high-purity high-activity iron oxide red as a raw material. The high-purity high-activity iron red requires the technical indexes of the iron red, such as the purity of more than 99.5 percent, the content of silicon dioxide of less than 0.1 percent, the content of chloride ions of less than 0.15 percent, and the like, has the average particle size of below 1 mu m, is fine powder with a hollow structure, and has large specific surface area and high reaction activity. Because the iron oxide red is a by-product of a steel mill in the recovery process of pickling waste liquor, the stability of the quality is not enough, the yield is greatly influenced by the capacity change of the steel mill, the situations of short supply and short demand and large market price fluctuation often occur, and particularly the iron oxide red for preparing high-grade permanent magnetic ferrite needs to depend on imported foreign high-quality iron oxide to meet corresponding technical indexes, so that the preparation of the high-grade permanent magnetic ferrite in China is limited, the competitiveness of the domestic and international markets is not enough, the yield of high-grade ferrite permanent magnetic materials with high added values is small, and the market share is low.
The iron ore concentrate has rich resources, relatively stable components and low price, and can be used as a raw material for preparing the permanent magnetic ferrite, but because the iron ore concentrate powder is solid particles, compared with iron red, the iron ore concentrate has thicker granularity, small specific surface area and poor reaction activity, and meanwhile, the iron ore concentrate mainly comprises ferroferric oxide, a considerable part of divalent iron ions which are not completely oxidized, and besides more silicon dioxide content (generally 0.5-1wt percent), other impurity elements exist. Therefore, it is difficult to prepare high-grade permanent magnetic ferrite permanent magnetic material by using iron concentrate powder as raw material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a method for preparing medium and high grade permanent magnetic ferrite by using iron concentrate powder as a raw material, breaks through the restriction of the raw material on the preparation of medium and high grade permanent magnetic ferrite materials, reduces the cost while obtaining the high performance permanent magnetic ferrite, and increases the market share of the high grade ferrite permanent magnetic material.
The invention discloses a method for preparing medium and high grade permanent magnetic ferrite by taking iron concentrate powder as a raw material, wherein the chemical structural formula of the permanent magnetic ferrite is R x Sr 1-x Fe 2n-y M y O 19 In the formula, x is more than or equal to 0.1 and less than or equal to 0.5, y is more than or equal to 0.1 and less than or equal to 0.4, n is more than or equal to 5.8 and less than or equal to 6.5, R is at least one of La, ce and Pr, M is at least one of Co, al and Zn, and the process steps are as follows:
(1) Ingredients
The permanent magnetic ferrite with the chemical structural formula is prepared, wherein the raw materials of the elements R and M are oxide powder of the permanent magnetic ferrite, and the raw material of the element Sr is SrCO 3 Powder, wherein the raw material of element Fe is iron concentrate powder, and the ingredients are prepared according to the chemical structural formula according to the content of total iron in the iron concentrate powder;
(2) Preparing a first slurry
The R oxide powder, the M oxide powder and the SrCO which are metered in the step (1) 3 Uniformly mixing the powder and iron ore concentrate powder to form mixed powder, adding a sintering aid A, a sintering aid B and water into the mixed powder, and performing wet ball milling to form first slurry with the average particle size of suspended particles of 0.6-1.0 mu m; the addition amount of the sintering aid A is 0.1-0.5% of the mass of the mixed powder, and the addition amount of the sintering aid B is 1-5% of the mass of the mixed powder;
(3) Preparation of permanent magnetic ferrite pre-sintering material
Filtering the first slurry obtained in the step (2), drying the wet material obtained by filtering, pre-burning the material obtained by drying at 1200-1300 ℃ for 2-4 h in air atmosphere, and cooling to room temperature along with the furnace to obtain a permanent magnetic ferrite pre-burnt material;
(4) Preparing the second slurry
Coarsely crushing and sieving the permanent magnetic ferrite pre-sintering material obtained in the step (3) to obtain pre-sintering material powder with the average particle size of 2-6 microns, then adding a surfactant, a secondary additive and water into the pre-sintering material powder, and performing wet ball milling to form second slurry with the average particle size of suspended particles of 0.6-1.0 microns; the addition amount of the surfactant is 0.1-2% of the mass of the pre-sintering material powder, and the addition amount of the secondary additive is 0.4-7% of the mass of the pre-sintering material powder;
(5) Preparation of the Green bodies
Filtering and dewatering the second slurry obtained in the step (4), controlling the water content of the wet material obtained after filtering and dewatering to be 35-45%, and then performing orientation pressing by adopting a wet pressing magnetic field to enable the wet material with the water content of 35-45% to form a green body, wherein the pulsed magnetic field is 6-10 KOe, and the pressing pressure is 7-9 MPa;
(6) Sintering
And (4) sintering the green body obtained in the step (5) in an air atmosphere at 1150-1300 ℃ for 0.5-3 h, and then cooling the green body to room temperature along with the furnace to obtain the medium-high grade permanent magnetic ferrite.
If the prepared permanent magnetic ferrite needs to be detected, a measurable standard block is obtained by grinding processing, and then the magnetic performance index is obtained by inspection and measurement according to the GB/T3217-92 national standard.
The invention relates to a method for preparing medium-high grade permanent magnetic ferrite by taking iron ore concentrate powder as a raw material, which comprises the following steps of (2) enabling a sintering aid A to consist of calcium carbonate powder and sodium hydroxide powder, wherein the mass ratio of the calcium carbonate powder to the sodium hydroxide powder is 1 (4.5-5.5); the sintering aid B consists of strontium chloride powder and potassium carbonate powder, and the mass ratio of the strontium chloride powder to the potassium carbonate powder is 1 (5.5-6.5).
The invention relates to a method for preparing medium and high grade permanent magnetic ferrite by using iron ore concentrate powder as a raw material, wherein in the step (4), the surfactant is at least one of glucose, calcium gluconate, sorbitol and polyethylene glycol; the secondary additive is CaCO 3 、SiO 2 、Al 2 O 3 、H 3 BO 3 、SrCO 3 、La 2 O 3 、Cr 2 O 3 At least the first three of the powders, caCO 3 The addition amount of the powder is 0.2-2% of the weight of the pre-sintering material powder, and SiO 2 The addition amount of the powder is 0.1-1% of the weight of the pre-sintering material powder, and Al 2 O 3 The addition amount of the powder is 0.1-1% of the weight of the pre-sintering material powder, and H 3 BO 3 The addition amount of the powder is 0 to 0.5 percent of the weight of the presintering material powder, and SrCO 3 The addition amount of the powder is 0 to 0.5 percent of the mass of the pre-sintering material powder, and La 2 O 3 The addition amount of the powder is 0-1% of the weight of the pre-sintering material powder, and Cr 2 O 3 The addition amount of the powder is 0-1% of the mass of the pre-sintering material powder.
The invention relates to a method for preparing medium and high grade permanent magnetic ferrite by using iron ore concentrate powder as a raw material, wherein in the step (3), the drying temperature of wet materials obtained by filtering is 150-200 ℃, and the drying time is 3-4 h.
The method for preparing the medium-high grade permanent magnetic ferrite by taking the iron ore concentrate powder as the raw material comprises the step (6) of controlling the heating rate of heating from room temperature to the sintering temperature of 1150-1300 ℃ to be 50-200 ℃/h.
The invention discloses a method for preparing medium and high grade permanent magnetic ferrite by using iron ore concentrate powder as a raw material, which comprises the steps of (2) and (4), wherein the wet ball milling is controlled according to the mass ratio of water to balls =1, (1.2-1.5) to (11.5-12.5).
The method of the invention can realize the mechanism explanation of preparing the medium-high grade permanent magnetic ferrite by taking iron concentrate powder as the raw material:
because the sintering aid A and the sintering aid B are added when the first slurry is prepared, in the pre-sintering process of preparing the permanent magnetic ferrite pre-sintering material from the wet material obtained by filtering the first slurry, the sintering aid A reacts with impurities such as silicon dioxide and the like to generate a silicate liquid phase with a low melting point, the liquid phase promotes the ion migration of a solid-liquid interface in the pre-sintering process, promotes the solid phase reaction activity in the ferrite transformation process, finally exists at the crystal boundary of the ferrite phase in the form of a bonding phase, and can promote the density of a magnet while inhibiting the growth of crystal grains, thereby promoting the coercive force and remanence of the magnet, and turning the influence of impurity elements on the permanent magnetic performance of the ferrite into good; the sintering aid B is a water-soluble substance, is adsorbed on the surface of the iron concentrate powder in the form of a molecular film, contains strontium element which reacts with the iron concentrate powder to generate a corresponding ferromagnetic phase, and generates a ferrite phase firstly in the process of presintering to promote the process of ferrite transformation, so that the problems of incomplete oxidation and poor reaction activity in the reaction process of the iron concentrate powder are solved, the solid phase reaction activity in the presintering process is promoted, the effective replacement of rare earth plasma in the presintering process is realized, and the rare earth plasma enters the permanent magnetic ferrite crystal lattice instead of existing in the crystal boundary of a non-magnetic phase.
Because the surfactant and the secondary additive are added when the second slurry is prepared, the surfactant can improve the particle agglomeration in the ball milling process, promote the ball milling refinement, promote the homogenization of the particle size of the pre-sintering material, and is beneficial to the improvement of the magnetic field orientation and the green body density in the process of preparing the green body from the wet material obtained by filtering the second slurry, the secondary additive can promote the solid phase sintering and improve the density and the strength of the magnet, and meanwhile, a liquid phase film is formed at the interface of the crystal grains of the magnet during the sintering, the growth of the crystal grains of the magnet is inhibited, and the comprehensive magnetic performance of the magnet is further improved.
The invention has the following beneficial effects:
1. according to the method, iron ore concentrate powder is used as a raw material of element Fe, a sintering aid A and a sintering aid B are added when first slurry is prepared, wet materials obtained by filtering the first slurry are presintered to form permanent magnetic ferrite presintered materials, then the presintered materials are crushed, a surfactant and a secondary additive are added, wet ball milling is carried out to form second slurry, green bodies prepared from the wet materials obtained by filtering the second slurry are sintered, and the residual magnetism Br is obtained: 420-430mT, coercive force HCB (hybrid magnetic resonance B) 285-310KA/m, intrinsic coercive force Hcj:340-370KA/m, maximum magnetic energy product BH (max) ：33-34KJ/m 3 The high magnetic performance permanent magnetic ferrite material breaks through the restriction of the raw materials on the preparation of middle and high grade permanent magnetic ferrite materials, is beneficial to enlarging the production scale of the middle and high grade permanent magnetic ferrite materials and improving the market share.
2. Because the method takes the iron concentrate powder as the raw material of the element Fe to prepare the high-magnetic-performance permanent magnetic ferrite material, the iron concentrate has rich resources and low price, and the cost can be reduced while the high-performance permanent magnetic ferrite is obtained.
3. The method of the invention does not need to add new equipment or modify the existing production equipment, thereby being beneficial to popularization.
Drawings
FIG. 1 is a graph of demagnetization of a permanent magnetic ferrite prepared in example 1;
FIG. 2 is a graph of demagnetization curves of the permanent magnetic ferrite prepared in example 2;
fig. 3 is a graph of demagnetization of the permanent magnetic ferrite prepared in example 3.
Detailed Description
The method for preparing the medium and high grade permanent magnetic ferrite by using the iron ore concentrate powder as the raw material according to the present invention is further described by the following embodiments and the accompanying drawings.
The iron ore concentrate used in the following examples was wei steel ore concentrate, and the mass fraction of total iron in the iron ore concentrate was 71.65%, the mass fraction of silica was 0.5%, and the mass fraction of alumina was 0.1%, as measured.
Example 1
The chemical structural formula of the permanent magnetic ferrite prepared in this example is Sr 0.8 La 0.2 Fe 11.5 Co 0.2 O 19 Wherein, X =0.2, y =0.2, n =5.85, and the process steps are as follows:
(1) Ingredients
The raw materials of the elements La and Co are respectively La 2 O 3 Powder, co 2 O 3 Powder, the raw material of element Sr is SrCO 3 Powder, wherein the raw material of element Fe is iron concentrate powder, and the ingredients are prepared according to the chemical structural formula according to the content of total iron in the iron concentrate powder; in the chemical structural formula, the molar ratio of each element is as follows: sr: la: fe: co =0.8:0.2:11.5:0.2, each raw material, srCO, was calculated and weighed in this molar ratio 3 Powder: 118.4g, la 2 O 3 Powder: 32.6g, iron ore concentrate powder: 899g, co 2 O 3 Powder: 16.6g;
(2) Preparing a first slurry
The measured SrCO in the step (1) 3 Powder, la 2 O 3 Powder, iron ore concentrate powder, co 2 O 3 Uniformly mixing the powder to form mixed powder, adding a sintering aid A, a sintering aid B and deionized water into the mixed powder, and performing wet ball milling to form first slurry, wherein the average particle size of suspended particles in the first slurry is 0.8 mu m; the sintering aid A consists of calcium carbonate powder and sodium hydroxide powder, the mass ratio of the calcium carbonate powder to the sodium hydroxide powder is 1; the sintering aid B consists of strontium chloride powder and potassium carbonate powder, the mass ratio of the strontium chloride powder to the potassium carbonate powder is 1; the roller ball mill for wet ball milling comprises the following materials: water: adding deionized water into the ball = 1.4;
(3) Preparation of permanent magnetic ferrite pre-sintering material
Filtering the first slurry obtained in the step (2), drying wet materials obtained by filtering at 200 ℃ for 4h in a muffle furnace, putting the materials obtained by drying into a roller kiln, pre-burning at 1280 ℃ for 3h in air atmosphere, and cooling to room temperature along with the furnace to obtain permanent magnetic ferrite pre-burning materials;
(4) Preparing the second slurry
Coarsely crushing the permanent magnetic ferrite pre-sintered material obtained in the step (3), sieving the pre-sintered material by a 120-mesh sieve to obtain pre-sintered material powder, adding a surfactant, a secondary additive and deionized water into the pre-sintered material powder, and performing wet ball milling to form second slurry with the average suspended particle size of 0.8 mu m; the surface active agent is sorbitol, the adding amount of the surface active agent is 0.6 percent of the mass of the pre-sintering material powder, and the secondary additive is CaCO 3 、SiO 2 、Al 2 O 3 、H 3 BO 3 And SrCO 3 ，CaCO 3 The addition amount of (B) is 0.6% of the weight of the pre-sintering material powder, and SiO 2 The addition amount of (C) is 0.3% of the weight of the pre-sintering material powder, and Al 2 O 3 The addition amount of (B) is 0.2% of the weight of the pre-sintering material powder, and H 3 BO 3 The addition amount of the sintering aid is 0.2 percent of the mass of the pre-sintering material powder, and SrCO 3 The addition amount of the pre-sintering material is 0.4 percent of the mass of the pre-sintering material powder; the roller ball mill for wet ball milling comprises the following materials: water: adding deionized water into the ball = 1.5;
(5) Preparation of the Green bodies
Filtering and dewatering the second slurry obtained in the step (4), controlling the water content of the wet material after filtering and dewatering to be 35%, and then adopting a wet-pressing magnetic field to carry out oriented pressing to obtain a green body with the diameter of 34.1mm and the height of 16mm, wherein the pulse magnetic field is 6KOe, and the pressing pressure is 8MPa;
(6) Sintering
And (5) putting the green body obtained in the step (5) into a roller kiln, heating the green body from room temperature to 1184 ℃ at the heating rate of 100 ℃/h, sintering the green body in the air atmosphere for 1h, and then cooling the green body to room temperature along with the furnace to obtain the permanent magnetic ferrite.
The permanent magnetic ferrite prepared in the embodiment is ground to obtain a measurable standard block, and magnetic property inspection and measurement are carried out according to the GB/T3217-92 national standardThe detection result is shown in a demagnetization curve shown in figure 1, and the residual magnetism Br is: 423mT, coercive force HCB 306KA/m, intrinsic coercive force Hcj:364KA/m, maximum energy product BH (max) ：33.8KJ/m 3 。
Example 2
The chemical structural formula of the permanent magnetic ferrite prepared in this example is Sr 0.65 La 0.3 Ce 0.05 Fe 12 Co 0.2 Zn 0.1 O 19 Wherein, X =0.35, y =0.3, n =6.1, and the process steps are as follows:
(1) Ingredients
The raw material of the element La is La 2 O 3 The powder and the element Ce are CeO 2 Powder, the raw material of the element Sr is SrCO 3 Powder, wherein the raw material of the element Fe is iron concentrate powder, and the raw material of the element Co is Co 2 O 3 The raw material of element Zn is ZnO powder, and the materials are proportioned according to the chemical structural formula according to the content of total iron in the iron concentrate powder; in the chemical structural formula, the molar ratio of each element is as follows: sr: la: ce: fe: co: zn =0.65:0.3:0.05:12:0.2:0.1, calculating and weighing the raw materials SrCO according to the molar ratio 3 Powder: 96.2g, la 2 O 3 Powder: 48.9g of CeO 2 Powder: 8.65g, iron concentrate powder: 938g, co 2 O 3 Powder: 16.6g, znO powder: 8.2g;
(2) Preparing a first slurry
The measured SrCO in the step (1) 3 Powder, la 2 O 3 Powder, ceO 2 Powder, iron ore concentrate powder, co 2 O 3 Uniformly mixing the powder and ZnO powder to form mixed powder, adding a sintering aid A, a sintering aid B and deionized water into the mixed powder, and performing wet ball milling to form first slurry, wherein the average particle size of suspended particles in the first slurry is 0.8 mu m; the sintering aid A consists of calcium carbonate powder and sodium hydroxide powder, the mass ratio of the calcium carbonate powder to the sodium hydroxide powder is 1; the sintering aid B consists of strontium chloride powder and potassium carbonate powder, the mass ratio of the strontium chloride powder to the potassium carbonate powder is 1(ii) a The roller ball mill for wet ball milling comprises the following materials: water: adding deionized water into the ball = 1.5;
(3) Preparation of permanent magnetic ferrite pre-sintering material
Filtering the first slurry obtained in the step (2), drying the wet material obtained by filtering at 180 ℃ for 4h in a muffle furnace, putting the material obtained by drying into a roller kiln, pre-sintering at 1300 ℃ for 2.5h in air atmosphere, and cooling to room temperature along with the furnace to obtain a permanent magnetic ferrite pre-sintered material;
(4) Preparing the second slurry
Coarsely crushing the permanent magnetic ferrite pre-sintered material obtained in the step (3), sieving the pre-sintered material by a 120-mesh sieve to obtain pre-sintered material powder, adding a surfactant, a secondary additive and deionized water into the pre-sintered material powder, and performing wet ball milling to form second slurry with the average suspended particle size of 0.8 mu m; the surfactant is calcium gluconate, the addition amount of the surfactant is 0.3 percent of the mass of the pre-sintering material powder, and the secondary additive is CaCO 3 、SiO 2 、Al 2 O 3 、H 3 BO 3 And La 2 O 3 ，CaCO 3 The addition amount of (B) is 0.6% of the weight of the pre-sintering material powder, and SiO 2 The addition amount of (C) is 0.3% of the weight of the pre-sintering material powder, and Al 2 O 3 The addition amount of (B) is 0.13% of the weight of the pre-sintering material powder, and H 3 BO 3 The addition amount of (A) is 0.2% of the weight of the pre-sintering material powder, and La 2 O 3 The addition amount of the additive is 0.4 percent of the mass of the pre-sintering material powder; the roller ball mill for wet ball milling comprises the following materials: water: adding deionized water according to the mass ratio of ball = 1.4;
(5) Preparation of the Green bodies
Filtering and dewatering the second slurry obtained in the step (4), controlling the water content of the wet material obtained after filtering and dewatering to be 40%, and then adopting a wet-pressing magnetic field orientation pressing method to form a green body with the diameter of 34.1mm and the height of 16mm, wherein the pulse magnetic field is 8KOe, and the pressing pressure is 8MPa;
(6) Sintering
And (5) placing the green body obtained in the step (5) into a roller kiln, heating the green body from room temperature to 1200 ℃ at the heating rate of 120 ℃/h, sintering the green body in the air atmosphere for 2h, and then cooling the green body to the room temperature along with the furnace to obtain the permanent magnetic ferrite.
The permanent magnetic ferrite prepared in the embodiment is ground to obtain a measurable standard block, magnetic property inspection and measurement are carried out according to the national standard GB/T3217-92, the detection result is shown in a demagnetization curve shown in figure 2, and the residual magnetism Br is: 429mT, coercive force HCB:289KA/m, intrinsic coercive force Hcj:343KA/m, maximum energy product BH (max) ：33.8KJ/m 3 。
Example 3
The chemical formula of the permanent magnetic ferrite prepared in this example is Sr 0.6 La 0.3 Pr 0.1 Fe 11.4 Co 0.2 Al 0.05 O 19 Wherein, X =0.4, y =0.25, n =5.825, and the process steps are as follows:
(1) Ingredients
The raw material of the element La is La 2 O 3 The raw material of the powder and the element Pr is Pr 6 O 11 Powder, the raw material of the element Sr is SrCO 3 Powder, wherein the raw material of the element Fe is iron concentrate powder, and the raw material of the element Co is Co 2 O 3 Powder, the raw material of the element Al is Al 2 O 3 The powder is prepared according to the chemical structural formula and the content of total iron in the iron concentrate powder; in the chemical structural formula, the molar ratio of each element is as follows: sr: la: pr: fe: co: al =0.6:0.3:0.1:11.4:0.2:0.05, each raw material, srCO, was calculated and weighed in this molar ratio 3 Powder: 89g, la 2 O 3 Powder: 48.9g, pr 6 O 11 Powder: 17g, iron concentrate powder: 892g, co 2 O 3 Powder: 16.6g of Al 2 O 3 Powder: 2.55g;
(2) Preparing a first slurry
The measured SrCO in the step (1) 3 Powder, la 2 O 3 Powder, pr 6 O 11 Powder, iron ore concentrate powder, co 2 O 3 Powder and Al 2 O 3 The powder is evenly mixed to form mixed powder, and then the sintering aid A, the sintering aid B and the deionization agent are added into the mixed powderWater, adopting wet ball milling to form first slurry, wherein the average particle size of suspended particles in the first slurry is 0.82 mu m; the sintering aid A consists of calcium carbonate powder and sodium hydroxide powder, the mass ratio of the calcium carbonate powder to the sodium hydroxide powder is 1; the sintering aid B consists of strontium chloride powder and potassium carbonate powder, the mass ratio of the strontium chloride powder to the potassium carbonate powder is 1; the roller ball mill for wet ball milling comprises the following materials: water: adding deionized water into the ball = 1.3;
(3) Preparation of permanent magnetic ferrite pre-sintering material
Filtering the first slurry obtained in the step (2), drying the wet material obtained by filtering at 200 ℃ for 3h in a muffle furnace, placing the material obtained by drying in a roller kiln, pre-sintering at 1250 ℃ for 3.5h in air atmosphere, and cooling to room temperature along with the furnace to obtain a permanent magnetic ferrite pre-sintered material;
(4) Preparing the second slurry
Coarsely crushing the permanent magnetic ferrite pre-sintered material obtained in the step (3), sieving the pre-sintered material by a 120-mesh sieve to obtain pre-sintered material powder, adding a surfactant, a secondary additive and deionized water into the pre-sintered material powder, and performing wet ball milling to form second slurry with the average suspended particle size of 0.85 mu m; the surfactant is polyethylene glycol, the addition amount of the surfactant is 0.5 percent of the mass of the pre-sintering material powder, and the secondary additive is CaCO 3 、SiO 2 、Al 2 O 3 、Cr 2 O 3 And La 2 O 3 ，CaCO 3 The addition amount of (A) is 0.6% of the weight of the pre-sintering material powder, and SiO is 2 The addition amount of (B) is 0.3% of the weight of the pre-sintering material powder, and Al 2 O 3 The addition amount of (B) is 0.13% of the weight of the pre-sintering material powder, and Cr 2 O 3 The addition amount of (B) is 0.2% of the weight of the pre-sintering material powder, and La 2 O 3 The addition amount of the pre-sintering material is 0.4 percent of the mass of the pre-sintering material powder; the roller ball mill for wet ball milling comprises the following materials: water: adding deionized water into the ball = 1.5;
(5) Preparation of the Green bodies
Filtering and dewatering the second slurry obtained in the step (4), controlling the water content of the wet material obtained after filtering and dewatering to be 45%, and then adopting a wet-pressing magnetic field orientation pressing method to form a green body with the diameter of 34.1mm and the height of 16mm, wherein the pulse magnetic field is 8KOe, and the pressing pressure is 9MPa;
(6) Sintering
And (5) putting the green body obtained in the step (5) into a roller kiln, heating the green body from room temperature to 1220 ℃ at the heating rate of 120 ℃/h, sintering the green body in an air atmosphere for 2h, and then cooling the green body to room temperature along with the furnace to obtain the permanent magnetic ferrite.
The permanent magnetic ferrite prepared in the embodiment is ground to obtain a measurable standard block, magnetic property inspection and measurement are carried out according to the GB/T3217-92 national standard, and the detection result is shown in a demagnetization curve shown in figure 3, and the residual magnetism Br is: 424mT, coercive force HCB 287KA/m, intrinsic coercive force Hcj:341KA/m, maximum energy product BH (max) ：33.64KJ/m 3 。
Claims (10)
1. A method for preparing a medium-high grade permanent magnetic ferrite by taking iron concentrate powder as a raw material is disclosed, wherein the chemical structural formula of the permanent magnetic ferrite is R x Sr 1-x Fe 2n-y M y O 19 In the formula, x is more than or equal to 0.1 and less than or equal to 0.5, y is more than or equal to 0.1 and less than or equal to 0.4, n is more than or equal to 5.8 and less than or equal to 6.5, R is at least one of La, ce and Pr, M is at least one of Co, al and Zn, and the method is characterized by comprising the following process steps:
(1) Ingredients
The permanent magnetic ferrite with the chemical structural formula is prepared, wherein the raw materials of elements R and M are oxide powder of the permanent magnetic ferrite, and the raw material of element Sr is SrCO 3 Powder, wherein the raw material of element Fe is iron concentrate powder, and the ingredients are prepared according to the chemical structural formula according to the content of total iron in the iron concentrate powder;
(2) Preparing a first slurry
The R oxide powder, the M oxide powder and the SrCO which are metered in the step (1) 3 Uniformly mixing the powder and iron ore concentrate powder to form mixed powder, adding a sintering aid A, a sintering aid B and water into the mixed powder, and performing wet ball milling to form first slurry with the average particle size of suspended particles of 0.6-1.0 mu m; the combustion assistant agentThe addition amount of A is 0.1-0.5% of the mass of the mixed powder, and the addition amount of the sintering aid B is 1-5% of the mass of the mixed powder;
(3) Preparation of permanent magnetic ferrite pre-sintering material
Filtering the first slurry obtained in the step (2), drying the wet material obtained by filtering, pre-burning the material obtained by drying at 1200-1300 ℃ for 2-4 h in air atmosphere, and cooling to room temperature along with the furnace to obtain a permanent magnetic ferrite pre-burning material;
(4) Preparing the second slurry
Coarsely crushing and sieving the permanent magnetic ferrite pre-sintering material obtained in the step (3) to obtain pre-sintering material powder with the average particle size of 2-6 microns, then adding a surfactant, a secondary additive and water into the pre-sintering material powder, and performing wet ball milling to form second slurry with the average particle size of suspended particles of 0.6-1.0 microns; the addition amount of the surfactant is 0.1-2% of the mass of the pre-sintering material powder, and the addition amount of the secondary additive is 0.4-7% of the mass of the pre-sintering material powder;
(5) Preparation of the Green bodies
Filtering and dewatering the second slurry obtained in the step (4), controlling the water content of the wet material obtained after filtering and dewatering to be 35-45%, and then performing orientation pressing by adopting a wet pressing magnetic field to enable the wet material with the water content of 35-45% to form a green body, wherein the pulsed magnetic field is 6-10 KOe, and the pressing pressure is 7-9 MPa;
(6) Sintering
And (4) sintering the green body obtained in the step (5) in an air atmosphere at 1150-1300 ℃ for 0.5-3 h, and then cooling to room temperature along with the furnace to obtain the medium-high grade permanent magnetic ferrite.
2. The method for preparing the medium-high grade permanent magnetic ferrite from the iron ore concentrate powder as the raw material according to claim 1, wherein in the step (2), the sintering aid A consists of calcium carbonate powder and sodium hydroxide powder, and the mass ratio of the calcium carbonate powder to the sodium hydroxide powder is 1 (4.5-5.5); the sintering aid B consists of strontium chloride powder and potassium carbonate powder, and the mass ratio of the strontium chloride powder to the potassium carbonate powder is 1 (5.5-6.5).
3. Root of herbaceous plantThe method for preparing the medium-high grade permanent magnetic ferrite from iron ore concentrate powder as claimed in claim 1 or 2, wherein in the step (4), the surfactant is at least one of glucose, calcium gluconate, sorbitol and polyethylene glycol; the secondary additive is CaCO 3 、SiO 2 、Al 2 O 3 、H 3 BO 3 、SrCO 3 、La 2 O 3 、Cr 2 O 3 At least the first three of the powders, caCO 3 The addition amount of the powder is 0.2-2% of the weight of the pre-sintering material powder, and SiO is added 2 The addition amount of the powder is 0.1-1% of the weight of the pre-sintering material powder, and Al 2 O 3 The addition amount of the powder is 0.1-1% of the weight of the pre-sintering material powder, and H 3 BO 3 The addition amount of the powder is 0 to 0.5 percent of the mass of the pre-sintering material powder, and SrCO 3 The addition amount of the powder is 0 to 0.5 percent of the weight of the pre-sintering material powder, and La 2 O 3 The addition amount of the powder is 0-1% of the weight of the pre-sintering material powder, and Cr 2 O 3 The addition amount of the powder is 0-1% of the weight of the pre-sintering material powder.
4. The method for preparing the medium and high grade permanent magnetic ferrite from iron ore concentrate powder as claimed in claim 1 or 2, wherein in the step (3), the drying temperature of the wet material obtained by filtering is 150-200 ℃ and the drying time is 3-4 h.
5. The method for preparing the medium and high grade permanent magnetic ferrite from iron ore concentrate powder as claimed in claim 3, wherein in the step (3), the drying temperature of the wet material obtained by filtering is 150-200 ℃ and the drying time is 3-4 h.
6. The method for preparing the medium-high grade permanent magnetic ferrite from iron ore concentrate powder as the raw material according to claim 1 or 2, wherein in the step (6), the heating rate from room temperature to the sintering temperature of 1150-1300 ℃ is controlled to be 50-200 ℃/h.
7. The method for preparing a medium-high grade permanent magnetic ferrite from iron ore concentrate powder as claimed in claim 3, wherein in the step (6), the temperature rise rate from room temperature to the sintering temperature of 1150-1300 ℃ is controlled to be 50-200 ℃/h.
8. The method for preparing medium and high grade permanent magnetic ferrite from iron ore concentrate powder as raw material according to claim 4, wherein in the step (6), the heating rate from room temperature to the sintering temperature of 1150-1300 ℃ is controlled to be 50-200 ℃/h.
9. The method for preparing medium and high grade permanent magnetic ferrite from iron ore concentrate powder as raw material according to claim 5, wherein in the step (6), the heating rate from room temperature to the sintering temperature of 1150-1300 ℃ is controlled to be 50-200 ℃/h.
10. The method for preparing the medium-high grade permanent magnetic ferrite by using the iron ore concentrate powder as the raw material according to claim 1 or 2, characterized in that in the step (2) and the step (4), the wet ball milling is controlled according to the mass ratio of water to balls =1 (1.2-1.5) to (11.5-12.5).
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