CN110128141A - A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method - Google Patents
A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method Download PDFInfo
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- CN110128141A CN110128141A CN201910494927.8A CN201910494927A CN110128141A CN 110128141 A CN110128141 A CN 110128141A CN 201910494927 A CN201910494927 A CN 201910494927A CN 110128141 A CN110128141 A CN 110128141A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
Abstract
The invention discloses a kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation methods, are related to rare earth permanent-magnetic material preparation and its applied technical field, are burnt in box by the way that graphite to be placed on sintering furnace and hold；Two layers of 40 molybdenum stainless (steel) wires are placed inside graphite；Novel sintered padding powder is sprinkled on 40 molybdenum stainless (steel) wires；Samarium-cobalt permanent-magnetic material is placed on the novel sintered use padding powder, and it is sintered.After the present invention is by using new underlayer, it eliminates high temperature and eliminates the zinc-plated process of the black cloth surface of 40 mesh, the viscous problem of bed course and samarium-cobalt permanent-magnetic material caused by the energy, the pollution for eliminating high-temperature processing device and processing are not thorough is saved, improve the qualification rate of product, be conducive to subsequent machining processes, after the powder for being sprinkled with a thin layer lanthanum oxide powder or samarium oxide powder or ceria oxide powder or the mixing of three's arbitrary proportion by stainless steel surface, thoroughly solve the problems, such as viscous.
Description
Technical field
The present invention relates to rare earth permanent-magnetic material manufacturing technology fields, and in particular to a kind of novel 2:17 type samarium-cobalt permanent-magnetic material
Sintering padding preparation method.
Background technique
2:17 type samarium-cobalt permanent-magnetic material has excellent temperature characterisitic and higher magnetic property, is widely used in aviation, boat
It, the fields such as defence and military, petroleum, specific type of electric machine, the production of 2:17 type sintered samarium cobalt magnetic material, which is divided into, smelts-powder-molding-burning processed
Five processes of knot-heat treatment, in sintering process, maximum temperature is up to 1210 degree, and material is at this temperature with the presence of liquid phase, therefore
The padding that blank is in contact with it frequent occurrence during the sintering process occurs to glue, and reduces the qualification rate of material, and seriously affect
The subsequent machining process of material.
Currently used padding is the 40 mesh Hei Sibu by high-temperature process, and overlay coating main component is metallic zinc,
It easily reacts with samarium-cobalt permanent-magnetic material under high temperature, influences the performance of material, so needing before use by high-temperature oxydation
Handle the zinc-plated of surface, on the one hand, high-temperature process waste of energy, pollution treatment device；On the other hand, the zinc-plated processing on surface is not
Thoroughly, still will affect the performance of samarium-cobalt permanent-magnetic material, this be current 2:17 type sintered samarium cobalt permanent-magnet material in process of production
One of predicament faced.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding systems
Preparation Method eliminates the viscous problem of bed course and samarium-cobalt permanent-magnetic material, improves product qualification rate, reduce production cost.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method, comprising the following steps:
(1) graphite is placed on sintering furnace and held and burnt in box；
(2) two layers of 40 molybdenum stainless (steel) wires are placed inside graphite；
(3) novel sintered padding powder is sprinkled on 40 molybdenum stainless (steel) wires；
(4) samarium-cobalt permanent-magnetic material is placed on the novel sintered use padding powder, and it is sintered.
Further, wherein novel sintered described in step 3 to use padding powder, it can be lithia, boron oxide, oxidation
Magnesium, aluminium oxide, silica, calcium oxide, scandium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, zinc oxide, gallium oxide, oxidation
Germanium, yttrium oxide, cerium oxide, praseodymium oxide, neodymia, samarium oxide, zirconium oxide, niobium oxide, molybdenum oxide, indium oxide, tin oxide, oxidation
At least one of hafnium, tantalum oxide, tungsten oxide, bismuth oxide, the powder that arbitrary proportion is mixed to get.
Still further, wherein novel sintered described in step 3 use padding powder, it can also be lithia, boron oxide, oxygen
Change magnesium, aluminium oxide, silica, calcium oxide, scandium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, zinc oxide, gallium oxide, oxygen
Change germanium, yttrium oxide, lanthana, praseodymium oxide, neodymia, samarium oxide, zirconium oxide, niobium oxide, molybdenum oxide, indium oxide, tin oxide, oxygen
Change at least one of hafnium, tantalum oxide, tungsten oxide, bismuth oxide, the powder that arbitrary proportion is mixed to get.
Still further, wherein novel sintered described in step 3 use padding powder, preferably lanthanum oxide powder or samarium oxide powder
The powder of end or the mixing of ceria oxide powder or three's arbitrary proportion, it is prepared by the following steps:
(1) lanthanum oxide powder La2O3Preparation
Take a certain amount of 0.1mol/L La (NO3)3Solution adds certain polyethylene glycol to stir evenly, is placed in 400ml beaker
It is heated on electric furnace, then 0.5mol/L NH is added dropwise4HCO3Solution, for control reaction temperature at 40 DEG C or so, PH is 7.0 or so.Reaction
After complete, it is aged 2h.Filtering is washed with a water washing, then with a small amount of dehydrated alcohol, up to lanthanum carbonate.Put the precipitate in baking
It in 70 DEG C of dry 1h in case, then is transferred in Muffle furnace and calcines 2h under certain temperature, ground using airflow milling, in argon atmosphere
In be crushed to average grain diameter be 10-60nm, aoxidize lanthanum oxide powder.
(2) samarium oxide powder Sm2O3Preparation
Take a certain amount of samaric nitrate (Sm (NO3)3·6H2O or samarium trichloride (SmCl3·6H2O it is) raw material, is dissolved in deionized water, matches
It is 0.1-0.3mol/L aqueous solution that concentration, which is made, is added drop-wise in (10% volume ratio) aqueous solution of 20-30% concentration ammonium hydroxide, and 2- is aged
3h is made Sm (OH)3Hydrogel.Then washing is sufficiently stirred with ionized water, filters and obtains filter cake, filter cake is empty at 110 DEG C
Gas or N2Dry 5-24h in gas, it is dry after sample at 500-600 DEG C air or N in Muffle furnace23-8h is roasted in gas, is adopted
It is ground with airflow milling, it is 1-5 μm that average grain diameter is crushed in argon atmosphere, samarium oxide fine catalyst.
(3) ceria oxide powder Ce2O3Preparation
By 2.3mmol Ce (NO3)3·6H2O, 0.27mmol Surfactant CTAB, 9.2mol urea are dissolved in the deionization of 10ml
It in water, is then put on magnetic stirring apparatus and stirs 15 minutes, dissolve solute all, obtain colorless and transparent solution.Again by it
Be transferred to 20m | inner liner polytetrafluoroethylene stainless steel autoclave in.It after sealing, is put into baking oven, it is added respectively
Heat to 120 ~ 180 °C, reaction 3h, 5h, 7h, 9h, 12h, for 24 hours, after 48h, cooled to room temperature.White obtained in it is heavy
It forms sediment centrifugation, and after washing 3 times with deionized water, dehydrated alcohol respectively, is put in 80 °C of baking ovens and dries 12h and obtain cerium oxide precursor
Body, that is, hexagonal crystal system CeOHCO3.After sample and this sample after reacting for 24 hours under 180 °C again calcine 10h under 500 °C
Sample.Presoma has been completely transformed into the CeO of cubic-crystal after calcining2, finally obtain the nano Ce O of 15-60nm2
Powder.
(4) three kinds of oxide mixing
The lanthana that will have been ground, samarium oxide, ceria oxide powder under an argon atmosphere be uniformly mixed obtain it is of the present invention novel
It is novel sintered to use padding powder.
Further, three kinds of oxide mixed methods use following steps:
(1) three kinds of oxides are sorted according to size, three kinds of oxides is separated into size rare earth up to standard
Oxide, size large particle rare-earth oxide and impurity not up to standard；
(2) by impurity from separating in large particle rare-earth oxide；
(3) large particle rare-earth oxide of separated impurity out is crushed, size after large particle rare-earth oxide is broken
Become smaller, and the impurity sticked on large particle rare-earth oxide also falls off in shattering process；
(4) large granular impurity after crushing in rare earth oxide is separated；
(5) rare earth oxide after isolating impurity in the step (4) is sorted again according to size, and size is reached
Target rare earth oxide separates the mixing for carrying out three kinds of oxides.
Further, in above-mentioned steps (1) and step (5), three kinds of oxides are sorted according to size
Equipment is high-efficiency fiber filter, and the high efficiency particulate air filter is using fiber as filtrate；
The component part of the high-efficiency fiber filter has fiber bundle media, fixed porous plate, active multi-hole plate, distribution device
Deng.
It further, is multiaxis self-action multiple-blade blender to the mixing arrangement of three kinds of oxides.
Further, the 90% of the novel sintered partial size with mixed oxide powder used in padding powder of the present invention
The above are 12 μm or less.
Further, it is of the present invention it is novel sintered in padding powder also containing platinum, gold, ruthenium, palladium and iridium at least one
Kind oxide.
Beneficial effects of the present invention: it after the present invention is by using new underlayer, eliminates high temperature and eliminates 40 mesh Hei Sibubiao
The zinc-plated process in face has saved the energy, has eliminated the pollution of high-temperature processing device and bed course and SmCo caused by processing is not thorough
The viscous problem of permanent-magnet material, improves the qualification rate of product, is conducive to subsequent machining processes, thoroughly solves the problems, such as viscous.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
A kind of Fig. 1: application drawing of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method.
Fig. 2: differential responses temperature oxidation lanthanum initial size.
Fig. 3: the SEM figure of cerium oxide nano in embodiment 1.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method, comprising the following steps:
(1) graphite is placed on sintering furnace and held and burnt in box；
(2) two layers of 40 molybdenum stainless (steel) wires are placed inside graphite；
(3) novel sintered padding powder is sprinkled on 40 molybdenum stainless (steel) wires；
(4) samarium-cobalt permanent-magnetic material is placed on novel sintered use padding powder, and it is sintered.
It is wherein novel sintered described in step 3 to use padding powder, it is prepared by the following steps:
(1) lanthanum oxide powder La2O3Preparation
Take a certain amount of 0.1mol/L La (NO3)3Solution adds certain polyethylene glycol to stir evenly, is placed in 400ml beaker
It is heated on electric furnace, then 0.5mol/L NH is added dropwise4HCO3Solution, for control reaction temperature at 40 DEG C or so, PH is 7.0 or so.Reaction
After complete, it is aged 2h.Filtering is washed with a water washing, then with a small amount of dehydrated alcohol, up to lanthanum carbonate.Put the precipitate in baking
It in 70 DEG C of dry 1h in case, then is transferred in Muffle furnace and calcines 2h under certain temperature, ground using airflow milling, in argon atmosphere
In be crushed to average grain diameter be 20-30nm, aoxidize lanthanum oxide powder.
(2) samarium oxide powder Sm2O3Preparation
Take a certain amount of samaric nitrate (Sm (NO3)3·6H2O or samarium trichloride (SmCl3·6H2O it is) raw material, is dissolved in deionized water, matches
It is 0.1-0.3mol/L aqueous solution that concentration, which is made, is added drop-wise in (10% volume ratio) aqueous solution of 20-30% concentration ammonium hydroxide, and 2- is aged
3h is made Sm (OH)3Hydrogel.Then washing is sufficiently stirred with ionized water, filters and obtains filter cake, filter cake is empty at 110 DEG C
Gas or N2Dry 5h in gas, it is dry after sample at 500 DEG C air or N in Muffle furnace28h is roasted in gas, is ground using airflow milling
Broken, it is 1-5 μm that average grain diameter is crushed in argon atmosphere, samarium oxide fine catalyst.
(3) ceria oxide powder Ce2O3Preparation
By 2.3mmol Ce (NO3)3·6H2O, 0.27mmol Surfactant CTAB, 9.2mol urea are dissolved in the deionization of 10ml
It in water, is then put on magnetic stirring apparatus and stirs 15 minutes, dissolve solute all, obtain colorless and transparent solution.Again by it
Be transferred to 20m | inner liner polytetrafluoroethylene stainless steel autoclave in.It after sealing, is put into baking oven, it is added respectively
Heat is to 180 °C, after reacting 3h, cooled to room temperature.By the centrifugation of white precipitate obtained in it, and respectively with deionized water,
After dehydrated alcohol washs 3 times, it is put in 80 °C of baking ovens dry 12h and obtains the cerium oxide precursor body i.e. CeOHCO of hexagonal crystal system3。
Sample and this sample after reacting for 24 hours under 180 °C again calcine the sample after 10h under 500 °C.Presoma is by calcining
Afterwards, it has been completely transformed into the CeO of cubic-crystal2, finally obtain the nano Ce O of 15nm2Powder.
(4) three kinds of oxide mixing
The lanthana that will have been ground, samarium oxide, ceria oxide powder are uniformly mixed obtain novel burning of the invention under an argon atmosphere
Knot padding powder.
Three kinds of oxide mixed methods use following steps:
(1) three kinds of oxides are sorted according to size, three kinds of oxides is separated into size rare earth up to standard
Oxide, size large particle rare-earth oxide and impurity not up to standard；
(2) by impurity from separating in large particle rare-earth oxide；
(3) large particle rare-earth oxide of separated impurity out is crushed, size after large particle rare-earth oxide is broken
Become smaller, and the impurity sticked on large particle rare-earth oxide also falls off in shattering process；
(4) large granular impurity after crushing in rare earth oxide is separated；
(5) rare earth oxide after isolating impurity in the step (4) is sorted again according to size, and size is reached
Target rare earth oxide separates the mixing for carrying out three kinds of oxides.
It according to the equipment that size is sorted is efficient to three kinds of oxides in above-mentioned steps (1) and step (5)
Fabric filter, the high efficiency particulate air filter is using fiber as filtrate；The component part of the high-efficiency fiber filter has fiber
Beam filtrate, fixed porous plate, active multi-hole plate, distribution device etc., the mixing arrangement to three kinds of oxides is that multiaxis is automatic
Formula multiple-blade blender.
Embodiment 2:
A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method, comprising the following steps:
(1) graphite is placed on sintering furnace and held and burnt in box；
(2) two layers of 40 molybdenum stainless (steel) wires are placed inside graphite；
(3) novel sintered padding powder is sprinkled on 40 molybdenum stainless (steel) wires；
(4) samarium-cobalt permanent-magnetic material is placed on the novel sintered use padding powder, and it is sintered.
It is wherein novel sintered described in step 3 to use padding powder, it is prepared by the following steps:
(1) lanthanum oxide powder La2O3Preparation
Take a certain amount of 0.1mol/L La (NO3)3Solution adds certain polyethylene glycol to stir evenly, is placed in 400ml beaker
It is heated on electric furnace, then 0.5mol/L NH is added dropwise4HCO3Solution, for control reaction temperature at 60 DEG C or so, PH is 7.0 or so.Reaction
After complete, it is aged 2h.Filtering is washed with a water washing, then with a small amount of dehydrated alcohol, up to lanthanum carbonate.Put the precipitate in baking
It in 70 DEG C of dry 1h in case, then is transferred in Muffle furnace and calcines 2h under certain temperature, ground using airflow milling, in argon atmosphere
In in be crushed to average grain diameter 30-50nm, aoxidize lanthanum oxide powder.
(2) samarium oxide powder Sm2O3Preparation
Take a certain amount of samaric nitrate (Sm (NO3)3·6H2O or samarium trichloride (SmCl3·6H2O it is) raw material, is dissolved in deionized water, matches
It is 0.1-0.3mol/L aqueous solution that concentration, which is made, is added drop-wise in (10% volume ratio) aqueous solution of 20-30% concentration ammonium hydroxide, and 2- is aged
3h is made Sm (OH)3Hydrogel.Then washing is sufficiently stirred with ionized water, filters and obtains filter cake, filter cake is empty at 110 DEG C
Gas or N2Dry 12h in gas, it is dry after sample at 550 DEG C air or N in Muffle furnace25h is roasted in gas, using airflow milling
Grind, in argon atmosphere in be crushed to average grain diameter be 1-5 μm, samarium oxide fine catalyst.
(3) ceria oxide powder Ce2O3Preparation
By 2.3mmol Ce (NO3)3·6H2O, 0.27mmol Surfactant CTAB, 9.2mol urea are dissolved in the deionization of 10ml
It in water, is then put on magnetic stirring apparatus and stirs 15 minutes, dissolve solute all, obtain colorless and transparent solution.Again by it
Be transferred to 20m | inner liner polytetrafluoroethylene stainless steel autoclave in.It after sealing, is put into baking oven, it is added respectively
Heat is to 160 °C, after reaction for 24 hours, cooled to room temperature.By the centrifugation of white precipitate obtained in it, and respectively with deionized water,
After dehydrated alcohol washs 3 times, it is put in 80 °C of baking ovens dry 12h and obtains the cerium oxide precursor body i.e. CeOHCO of hexagonal crystal system3。
Sample and this sample after reacting for 24 hours under 180 °C again calcine the sample after 10h under 500 °C.Presoma is by calcining
Afterwards, it has been completely transformed into the CeO of cubic-crystal2, finally obtain the nano Ce O of 30nm2Powder.
(4) three kinds of oxide mixing
The lanthana that will have been ground, samarium oxide, ceria oxide powder are uniformly mixed obtain novel burning of the invention under an argon atmosphere
Knot padding powder.
Three kinds of oxide mixed methods use following steps:
(1) three kinds of oxides are sorted according to size, three kinds of oxides is separated into size rare earth up to standard
Oxide, size large particle rare-earth oxide and impurity not up to standard；
(2) by impurity from separating in large particle rare-earth oxide；
(3) large particle rare-earth oxide of separated impurity out is crushed, size after large particle rare-earth oxide is broken
Become smaller, and the impurity sticked on large particle rare-earth oxide also falls off in shattering process；
(4) large granular impurity after crushing in rare earth oxide is separated；
(5) rare earth oxide after isolating impurity in the step (4) is sorted again according to size, and size is reached
Target rare earth oxide separates the mixing for carrying out three kinds of oxides.
It according to the equipment that size is sorted is efficient to three kinds of oxides in above-mentioned steps (1) and step (5)
Fabric filter, the high efficiency particulate air filter is using fiber as filtrate；The component part of the high-efficiency fiber filter has fiber
Beam filtrate, fixed porous plate, active multi-hole plate, distribution device etc., the mixing arrangement to three kinds of oxides is that multiaxis is automatic
Formula multiple-blade blender.
Embodiment 3:
A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method, comprising the following steps:
(1) graphite is placed on sintering furnace and held and burnt in box；
(2) two layers of 40 molybdenum stainless (steel) wires are placed inside graphite；
(3) novel sintered padding powder is sprinkled on 40 molybdenum stainless (steel) wires；
(4) samarium-cobalt permanent-magnetic material is placed on the novel sintered use padding powder, and it is sintered.
It is wherein novel sintered described in step 3 to use padding powder, it is characterised in that be prepared by the following steps:
(1) lanthanum oxide powder La2O3Preparation
Take a certain amount of 0.1mol/L La (NO3)3Solution adds certain polyethylene glycol to stir evenly, is placed in 400ml beaker
It is heated on electric furnace, then 0.5mol/L NH is added dropwise4HCO3Solution, for control reaction temperature at 80 DEG C or so, PH is 7.0 or so.Reaction
After complete, it is aged 2h.Filtering is washed with a water washing, then with a small amount of dehydrated alcohol, up to lanthanum carbonate.Put the precipitate in baking
It in 70 DEG C of dry 1h in case, then is transferred in Muffle furnace and calcines 2h under certain temperature, ground using airflow milling, in argon atmosphere
In be crushed to average grain diameter be 40-60nm, aoxidize lanthanum oxide powder.
(2) samarium oxide powder Sm2O3Preparation
Take a certain amount of samaric nitrate (Sm (NO3)3·6H2O or samarium trichloride (SmCl3·6H2O it is) raw material, is dissolved in deionized water, matches
It is 0.1-0.3mol/L aqueous solution that concentration, which is made, is added drop-wise in (10% volume ratio) aqueous solution of 20-30% concentration ammonium hydroxide, and 2- is aged
3h is made Sm (OH)3Hydrogel.Then washing is sufficiently stirred with ionized water, filters and obtains filter cake, filter cake is empty at 110 DEG C
Gas or N2In gas it is dry for 24 hours, it is dry after sample at 600 DEG C air or N in Muffle furnace23h is roasted in gas, using airflow milling
It grinds, it is 1-5 μm that average grain diameter is crushed in argon atmosphere, samarium oxide fine catalyst.
(3) ceria oxide powder Ce2O3Preparation
By 2.3mmol Ce (NO3)3·6H2O, 0.27mmol Surfactant CTAB, 9.2mol urea are dissolved in the deionization of 10ml
It in water, is then put on magnetic stirring apparatus and stirs 15 minutes, dissolve solute all, obtain colorless and transparent solution.Again by it
Be transferred to 20m | inner liner polytetrafluoroethylene stainless steel autoclave in.It after sealing, is put into baking oven, it is added respectively
Heat is to 140 °C, after reacting 48h, cooled to room temperature.By the centrifugation of white precipitate obtained in it, and respectively with deionized water,
After dehydrated alcohol washs 3 times, it is put in 80 °C of baking ovens dry 12h and obtains the cerium oxide precursor body i.e. CeOHCO of hexagonal crystal system3。
Sample and this sample after reacting for 24 hours under 180 °C again calcine the sample after 10h under 500 °C.Presoma is by calcining
Afterwards, it has been completely transformed into the CeO of cubic-crystal2, finally obtain the nano Ce O of 60nm2Powder.
(4) three kinds of oxide mixing
The lanthana that will have been ground, samarium oxide, ceria oxide powder are uniformly mixed obtain novel burning of the invention under an argon atmosphere
Knot padding powder.
Three kinds of oxide mixed methods use following steps:
(1) three kinds of oxides are sorted according to size, three kinds of oxides is separated into size rare earth up to standard
Oxide, size large particle rare-earth oxide and impurity not up to standard；
(2) by impurity from separating in large particle rare-earth oxide；
(3) large particle rare-earth oxide of separated impurity out is crushed, size after large particle rare-earth oxide is broken
Become smaller, and the impurity sticked on large particle rare-earth oxide also falls off in shattering process；
(4) large granular impurity after crushing in rare earth oxide is separated；
(5) rare earth oxide after isolating impurity in the step (4) is sorted again according to size, and size is reached
Target rare earth oxide separates the mixing for carrying out three kinds of oxides.
It according to the equipment that size is sorted is efficient to three kinds of oxides in above-mentioned steps (1) and step (5)
Fabric filter, the high efficiency particulate air filter is using fiber as filtrate；The component part of the high-efficiency fiber filter has fiber
Beam filtrate, fixed porous plate, active multi-hole plate, distribution device etc., the mixing arrangement to three kinds of oxides is that multiaxis is automatic
Formula multiple-blade blender.
To sum up, 2:17 type samarium-cobalt permanent-magnetic material sintering padding of the invention eliminates high temperature and eliminates the black cloth surface of 40 mesh
Zinc-plated process, saved the energy, eliminate the pollution of high-temperature processing device and bed course and SmCo caused by processing is not thorough forever
The viscous problem of magnetic material, improves the qualification rate of product, is conducive to subsequent machining processes, thoroughly solves the problems, such as viscous.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method, which comprises the following steps:
(1) graphite is placed on sintering furnace and held and burnt in box；
(2) two layers of 40 molybdenum stainless (steel) wires are placed inside graphite；
(3) novel sintered padding powder is sprinkled on 40 molybdenum stainless (steel) wires；
(4) samarium-cobalt permanent-magnetic material is placed on the novel sintered use padding powder, and it is sintered.
2. a kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method according to claim 1, feature
It is that novel sintered described in step 3 with padding powder is oxide, it is characterised in that oxide can be lithia, oxidation
Boron, magnesia, aluminium oxide, silica, calcium oxide, scandium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, zinc oxide, oxidation
Gallium, germanium oxide, yttrium oxide, cerium oxide, praseodymium oxide, neodymia, samarium oxide, zirconium oxide, niobium oxide, molybdenum oxide, indium oxide, oxidation
At least one of tin, hafnium oxide, tantalum oxide, tungsten oxide, bismuth oxide, the powder that arbitrary proportion is mixed to get.
3. a kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method according to claim 1, feature
Be described in step 3 it is novel sintered use padding powder, it is characterised in that oxide can for lithia, boron oxide, magnesia,
Aluminium oxide, silica, calcium oxide, scandium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, zinc oxide, gallium oxide, germanium oxide,
Yttrium oxide, lanthana, praseodymium oxide, neodymia, samarium oxide, zirconium oxide, niobium oxide, molybdenum oxide, indium oxide, tin oxide, hafnium oxide,
At least one of tantalum oxide, tungsten oxide, bismuth oxide, the powder that arbitrary proportion is mixed to get.
4. a kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method according to claim 1, feature
Be it is novel sintered described in step 3 use padding powder, can by lanthanum oxide powder or samarium oxide powder or ceria oxide powder or
The powder of three's arbitrary proportion mixing, it is characterised in that be prepared by the following steps:
(1) lanthanum oxide powder La2O3Preparation
Take a certain amount of 0.1mol/L La (NO3)3Solution adds certain polyethylene glycol to stir evenly, is placed on electricity in 400ml beaker
It is heated on furnace, then 0.5mol/L NH is added dropwise4HCO3Solution, for control reaction temperature at 40 DEG C or so, PH is 7.0 or so；
After having reacted, it is aged 2h；
Filtering is washed with a water washing, then with a small amount of dehydrated alcohol, up to lanthanum carbonate；
It puts the precipitate in 70 DEG C of dry 1h in baking oven, then is transferred in Muffle furnace and calcines 2h under certain temperature, using air-flow
Mill is ground, and it is 1-5 μm that average grain diameter is crushed in argon atmosphere, aoxidizes lanthanum oxide powder；
(2) samarium oxide powder Sm2O3Preparation
Take a certain amount of samaric nitrate (Sm (NO3)3·6H2O or samarium trichloride (SmCl3·6H2O it is) raw material, is dissolved in deionized water, matches
It is 0.1-0.3mol/L aqueous solution that concentration, which is made, is added drop-wise in (10% volume ratio) aqueous solution of 20-30% concentration ammonium hydroxide, and 2- is aged
3h is made Sm (OH)3Hydrogel；
Then with ionized water be sufficiently stirred washing, filter obtain filter cake, by filter cake at 110 DEG C air or N2Dry 5- in gas
For 24 hours, sample after dry air or N in Muffle furnace at 500-600 DEG C23-8h is roasted in gas, is ground using airflow milling,
It is 1-5 μm that average grain diameter is crushed in argon atmosphere, samarium oxide fine catalyst；
(3) ceria oxide powder Ce2O3Preparation
By 2.3mmol Ce (NO3)3·6H2O, 0.27mmol Surfactant CTAB, 9.2mol urea are dissolved in the deionization of 10ml
It in water, is then put on magnetic stirring apparatus and stirs 15 minutes, dissolve solute all, obtain colorless and transparent solution；
Be transferred into 20m again | inner liner polytetrafluoroethylene stainless steel autoclave in；
After sealing, be put into baking oven, be separately heated to 120 ~ 180 °C, reaction 3h, 5h, 7h, 9h, 12h, for 24 hours, after 48h,
Cooled to room temperature；
By the centrifugation of white precipitate obtained in it, and after washing 3 times with deionized water, dehydrated alcohol respectively, it is put in 80 °C of baking ovens
Middle dry 12h obtains the cerium oxide precursor body i.e. CeOHCO of hexagonal crystal system3；
Sample and this sample after reacting for 24 hours under 180 °C again calcine the sample after 10h under 500 °C；
Presoma has been completely transformed into the CeO of cubic-crystal after calcining2, finally obtain the nano Ce O of 15-60nm2Powder
Body；
(4) three kinds of oxide mixing
The lanthana that will have been ground, samarium oxide, ceria oxide powder be uniformly mixed under an argon atmosphere obtain it is described novel sintered
With padding powder.
5. a kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method according to claim 4 is novel sintered
With padding powder, which is characterized in that it is described it is novel sintered use padding powder, by the lanthanum oxide powder or samarium oxide powder or
Ceria oxide powder or the powder thickness of three's arbitrary proportion mixing are 10 ~ 50nm.
6. -5 any novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method, feature exist according to claim 1
In the novel sintered padding powder, i.e. lanthanum oxide powder or samarium oxide powder or ceria oxide powder or three's arbitrary proportion
Application of the mixed powder in manufacturing technique of permanent-magnet material field.
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| CN115138843A (en) * | 2022-06-29 | 2022-10-04 | 包头金山磁材有限公司 | Neodymium iron boron sintering material box and preparation method and application thereof |
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