CN108320899A - A kind of chemical treatment method on magnetic powder surface - Google Patents
A kind of chemical treatment method on magnetic powder surface Download PDFInfo
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- CN108320899A CN108320899A CN201810276813.1A CN201810276813A CN108320899A CN 108320899 A CN108320899 A CN 108320899A CN 201810276813 A CN201810276813 A CN 201810276813A CN 108320899 A CN108320899 A CN 108320899A
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- magnetic powder
- chemical treatment
- treatment method
- silane coupling
- coupling agent
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/02—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Magnetic Record Carriers (AREA)
- Developing Agents For Electrophotography (AREA)
Abstract
The invention discloses a kind of chemical treatment methods on magnetic powder surface, include the following steps:S1, untreated magnetic powder is added in reaction bulb, reenters 4A molecular sieves and ethyl alcohol, ultrasound and reduced pressure treatment, filtered, centrifuge after ultrasound, being concentrated under reduced pressure up to dehydration magnetic powder;S2, the surface conditioning agent mixed by silane coupling agent, diethylene glycol monolaurate and polyoxypropylene mannitol dioleate is added into dehydration magnetic powder, seals, shake, centrifugation, and liquid is discarded supernatant, then precipitation is dried in vacuo, it crushes, is sieved up to the magnetic powder after chemical treatment.Magnetic powder processing method proposed by the present invention, in such a way that degassing and chemical treatment are combined, chemically treated influence of the presence of magnetic powder surface moisture and air on the later stage can effectively be avoided, the surface lipophile that magnetic powder can also be significantly improved in the case where ensureing that magnetic powder self performance is without damage simultaneously, improves the dispersion performance of magnetic powder.
Description
Technical field
The present invention relates to magnetic powder processing technology field more particularly to a kind of chemical treatment methods on magnetic powder surface.
Background technology
Magnetic powder is a kind of single domain particle of hard magnetic, and magnetic paint is mixed and made into adhesive, solvent etc., can be coated in modeling
The magnetic recording materials such as tape, disk, magnetic card are made in the surface of material or metal chip base, are widely used in broadcast, TV, electronics
Computer, data preservation and ticket etc..However air and moisture are easily adsorbed in untreated magnetic powder surface, are not easy
It is combined with oleophilic substance, causes the dispersion effect between magnetic powder and adhesive equal solvent poor, influenced magnetic powder and play its basic training
Energy.In order to improve the oleophylic performance on magnetic powder surface, handled on magnetic powder surface usually using coupling agent, however existing coupling
When handling magnetic powder surface, the effect is unsatisfactory for agent, needs 200~500 DEG C of high temperature or is used for multiple times strongly mixed
Conjunction machine carries out forcing absorption, is both impacted to the performance of magnetic powder itself, while increasing intractability, reduces processing effect
Rate.Based on the shortcomings of the prior art, the present invention proposes a kind of chemical treatment method on magnetic powder surface.
Invention content
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of chemistry on the magnetic powder surface proposed
Processing method.
A kind of chemical treatment method on magnetic powder surface, includes the following steps:
The dehydration of S1, magnetic powder:Untreated magnetic powder is weighed, and is added in reaction bulb, then 4A points are added into reaction bulb
Son sieve and ethyl alcohol, then will connect vacuum pump, and reaction bulb is placed in Ultrasound Instrument on reaction bulb, 10~30min of ultrasound, and
Open vacuum pump while ultrasonic, carry out reduced pressure treatment, after ultrasound through filtering, centrifugation, be concentrated under reduced pressure up to dehydration magnetic powder;
The chemical treatment of S2, magnetic powder:It is added into dehydration magnetic powder by silane coupling agent, diethylene glycol monolaurate and polyoxy third
The surface conditioning agent that alkene mannitol dioleate mixes, and sealing, transfer to concussion 30 in concussion instrument~
60min after concussion, takes out, centrifugation, and discards supernatant liquid, is then dried in vacuo precipitation, crushes, and is sieved up to chemistry
Treated magnetic powder.
Preferably, the addition quality of 4A molecular sieves is 0.5~0.8 times of magnetic powder in the step S1, the addition of ethyl alcohol
It it is 5~8 times of magnetic powder and 4A molecular sieve gross masses, the water content in the ethyl alcohol is less than 2%, and the ethyl alcohol is that chemistry is pure, analysis
Any one in pure or chromatographically pure.
Preferably, frequency ultrasonic in the step S1 is 40~100KHZ, and water temperature control is 10~30 when described ultrasonic
℃。
Preferably, the speed centrifuged in the step S1 and step S2 be 3000~5000r/min, centrifugation time be 15~
20min。
Preferably, the weight of the silane coupling agent, diethylene glycol monolaurate and polyoxypropylene mannitol dioleate
It is 8~12 that amount part, which is compared,:3~6:3~6, it is further preferred that the silane coupling agent, diethylene glycol monolaurate and polyoxy
The weight part ratio of propylene mannitol dioleate is 2:1:1.
Preferably, the preparation method of the surface conditioning agent is:By diethylene glycol monolaurate and polyoxypropylene sweet dew
Alcohol dioleate is added in silane coupling agent, and stirs 15~25min in 40~60 DEG C, then keeps the temperature 30~40min, then cold
But to room temperature up to surface conditioning agent.
Preferably, the silane coupling agent is that the volume in Silane coupling agent KH550 or silane coupling agent KH560 is any one
Kind, and the content of silane coupling agent is more than 98%.
Preferably, water temperature when being shaken in the step S2 in concussion instrument is 30~50 DEG C, amplitude 20mm, and rotating speed is
100~300r/min.
Preferably, vacuum drying temperature is 98~108 DEG C in the step S2.
Magnetic powder surface treatment method proposed by the present invention can be effective in such a way that degassing and chemical treatment are combined
Avoid chemically treated influence of the presence of magnetic powder surface moisture and air on the later stage, at the same ensure magnetic powder self performance not by
The surface lipophile that magnetic powder can also be significantly improved in the case of damage improves the dispersion performance of magnetic powder, and at degassing and chemistry
Managing the mode being combined has complementary effect, and the two, which is jointly processed by, can have the dispersibility of magnetic powder significant promote
Effect, when being carried out dehydrating, magnetic powder is jointly processed by using 4A molecular sieves and ethyl alcohol, can be adsorbed on the water on magnetic powder surface
In 4A molecular sieves, moreover it is possible in ethanol by residual moisture dissolving, using ultrasound and reduced pressure treatment, magnetic powder surface can be adhered to
Air removal, finally using the processing of the surface conditioning agent of special preparation, magnetic powder can be significantly improved in oily matter
Dispersibility, surface conditioning agent is with the silane coupling agent of rational proportion, diethylene glycol monolaurate and polyoxypropylene mannitol
Dioleate mixes, and three, which cooperates, can be effectively improved the dispersibility on magnetic powder surface, and seals, concussion, centrifuges
Operation can be such that magnetic powder and surface conditioning agent effectively combines, and further increase the dispersibility of magnetic powder.
Specific implementation mode
The present invention is made further to explain with reference to specific embodiment.
Embodiment one
A kind of chemical treatment method on magnetic powder surface proposed by the present invention, includes the following steps:
The dehydration of S1, magnetic powder:Untreated magnetic powder is weighed, and is added in reaction bulb, then 0.6 times is added into reaction bulb
Then the 4A molecular sieves and ethyl alcohol of amount will connect vacuum pump, and reaction bulb are placed in Ultrasound Instrument on reaction bulb, ultrasonic 20min,
And the frequency of ultrasound is 80KHZ, water temperature control is at 10~30 DEG C when ultrasonic, and opens vacuum pump while ultrasound, is subtracted
Pressure is handled, and through filtering after ultrasound, then with the speed centrifugation 20min of 4000r/min, then is concentrated under reduced pressure up to magnetic powder is dehydrated;
The chemical treatment of S2, magnetic powder:To dehydration magnetic powder in be added by Silane coupling agent KH550, diethylene glycol monolaurate and
The surface conditioning agent that polyoxypropylene mannitol dioleate mixes, and seal, it transfers in concussion instrument and shakes
45min, and the water temperature in concussion instrument is 40 DEG C, amplitude 20mm, rotating speed 200r/min, after concussion, is taken out, with
The speed of 4000r/min centrifuges 20min, and discards supernatant liquid, then will be deposited in 102 DEG C of vacuum drying, crushes, is sieved to obtain the final product
Magnetic powder after chemical treatment.
In the present invention, the addition of ethyl alcohol is 6 times of magnetic powder and 4A molecular sieve gross masses, and ethyl alcohol is that chemistry is pure;Silane is even
The weight part ratio for joining agent KH550, diethylene glycol monolaurate and polyoxypropylene mannitol dioleate is 10:5:4;At surface
Reason agent preparation method be:Diethylene glycol monolaurate and polyoxypropylene mannitol dioleate are added to silane coupling agent
In KH550, and 25min is stirred in 50 DEG C, then keep the temperature 35min, then cooled to room temperature up to surface conditioning agent.
Embodiment two
A kind of chemical treatment method on magnetic powder surface proposed by the present invention, includes the following steps:
The dehydration of S1, magnetic powder:Untreated magnetic powder is weighed, and is added in reaction bulb, then 0.8 times is added into reaction bulb
Then the 4A molecular sieves and ethyl alcohol of amount will connect vacuum pump, and reaction bulb are placed in Ultrasound Instrument on reaction bulb, ultrasonic 15min,
And the frequency of ultrasound is 40KHZ, water temperature control is at 10~30 DEG C when ultrasonic, and opens vacuum pump while ultrasound, is subtracted
Pressure is handled, and through filtering after ultrasound, then with the speed centrifugation 20min of 5000r/min, then is concentrated under reduced pressure up to magnetic powder is dehydrated;
The chemical treatment of S2, magnetic powder:To dehydration magnetic powder in be added by silane coupling agent KH560, diethylene glycol monolaurate and
The surface conditioning agent that polyoxypropylene mannitol dioleate mixes, and seal, it transfers in concussion instrument and shakes
40min, and the water temperature in concussion instrument is 30 DEG C, amplitude 20mm, rotating speed 300r/min, after concussion, is taken out, with
The speed of 5000r/min centrifuges 20min, and discards supernatant liquid, then will be deposited in 108 DEG C of vacuum drying, crushes, is sieved to obtain the final product
Magnetic powder after chemical treatment.
In the present invention, the addition of ethyl alcohol is 5 times of magnetic powder and 4A molecular sieve gross masses, and ethyl alcohol is that analysis is pure;Silane is even
The weight part ratio for joining agent KH560, diethylene glycol monolaurate and polyoxypropylene mannitol dioleate is 8:3:5;At surface
Reason agent preparation method be:Diethylene glycol monolaurate and polyoxypropylene mannitol dioleate are added to silane coupling agent
In KH560, and 15min is stirred in 60 DEG C, then keep the temperature 40min, then cooled to room temperature up to surface conditioning agent.
Embodiment three
A kind of chemical treatment method on magnetic powder surface proposed by the present invention, includes the following steps:
The dehydration of S1, magnetic powder:Untreated magnetic powder is weighed, and is added in reaction bulb, then 0.6 times is added into reaction bulb
Then the 4A molecular sieves and ethyl alcohol of amount will connect vacuum pump, and reaction bulb are placed in Ultrasound Instrument on reaction bulb, ultrasonic 30min,
And the frequency of ultrasound is 80KHZ, water temperature control is at 10~30 DEG C when ultrasonic, and opens vacuum pump while ultrasound, is subtracted
Pressure is handled, and through filtering after ultrasound, then with the speed centrifugation 18min of 4000r/min, then is concentrated under reduced pressure up to magnetic powder is dehydrated;
The chemical treatment of S2, magnetic powder:To dehydration magnetic powder in be added by Silane coupling agent KH550, diethylene glycol monolaurate and
The surface conditioning agent that polyoxypropylene mannitol dioleate mixes, and seal, it transfers in concussion instrument and shakes
45min, and the water temperature in concussion instrument is 40 DEG C, amplitude 20mm, rotating speed 200r/min, after concussion, is taken out, with
The speed of 4000r/min centrifuges 18min, and discards supernatant liquid, then will be deposited in 103 DEG C of vacuum drying, crushes, is sieved to obtain the final product
Magnetic powder after chemical treatment.
In the present invention, the addition of ethyl alcohol is 6 times of magnetic powder and 4A molecular sieve gross masses, and ethyl alcohol is that chemistry is pure;Silane is even
The weight part ratio for joining agent KH550, diethylene glycol monolaurate and polyoxypropylene mannitol dioleate is 2:1:1;At surface
Reason agent preparation method be:Diethylene glycol monolaurate and polyoxypropylene mannitol dioleate are added to silane coupling agent
In KH550, and 20min is stirred in 50 DEG C, then keep the temperature 35min, then cooled to room temperature up to surface conditioning agent.
Comparative example one
Magnetic powder after dehydration is directly dried in vacuo, powder by the chemical treatment compared to embodiment one without magnetic powder
Broken and sieving processing.
Comparative example two
Untreated magnetic powder is directly added surface conditioning agent, and pressed by the dehydration compared to embodiment one without magnetic powder
According to step S2 processing in embodiment one.
In above-described embodiment one to embodiment three, the water content of ethyl alcohol is less than 2%, and the content of silane coupling agent is more than 98%.
To above-described embodiment one, embodiment two, embodiment three, comparative example one, treated the magnetic powder of comparative example two and not
Processed magnetic powder carries out dispersed detection, and is standard with the jitter time of untreated magnetic powder, calculates jitter time
Change percentage, it is as a result as follows:
As a result it shows:The dispersibility of embodiment one, embodiment two, embodiment three, comparative example one, comparative example two treated magnetic powder
Dispersibility relative to untreated magnetic powder has improvement, and the improvement of embodiment one, embodiment two, embodiment three will be got well
In comparative example one and comparative example two, show:The dehydration of magnetic powder proposed by the present invention and chemical treatment can be to magnetic powders
Dispersibility is with facilitation, and simultaneously used time dispersion effect improves significantly for dehydration and chemical treatment.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of chemical treatment method on magnetic powder surface, which is characterized in that include the following steps:
The dehydration of S1, magnetic powder:Untreated magnetic powder is weighed, and is added in reaction bulb, then 4A points are added into reaction bulb
Son sieve and ethyl alcohol, then will connect vacuum pump, and reaction bulb is placed in Ultrasound Instrument on reaction bulb, 10~30min of ultrasound, and
Open vacuum pump while ultrasonic, carry out reduced pressure treatment, after ultrasound through filtering, centrifugation, be concentrated under reduced pressure up to dehydration magnetic powder;
The chemical treatment of S2, magnetic powder:It is added into dehydration magnetic powder by silane coupling agent, diethylene glycol monolaurate and polyoxy third
The surface conditioning agent that alkene mannitol dioleate mixes, and sealing, transfer to concussion 30 in concussion instrument~
60min after concussion, takes out, centrifugation, and discards supernatant liquid, is then dried in vacuo precipitation, crushes, and is sieved up to chemistry
Treated magnetic powder.
2. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that 4A in the step S1
The addition quality of molecular sieve is 0.5~0.8 times of magnetic powder, and the addition of ethyl alcohol is the 5~8 of magnetic powder and 4A molecular sieve gross masses
Times, water content in the ethyl alcohol is less than 2%, and the ethyl alcohol is that chemistry is pure, analyzes any one in pure or chromatographically pure.
3. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that surpass in the step S1
The frequency of sound is 40~100KHZ, and water temperature control is at 10~30 DEG C when described ultrasonic.
4. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that the step S1 and step
The speed centrifuged in rapid S2 is 3000~5000r/min, and centrifugation time is 15~20min.
5. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that described silane coupled
The weight part ratio of agent, diethylene glycol monolaurate and polyoxypropylene mannitol dioleate is 8~12:3~6:3~6.
6. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that the surface conditioning agent
Preparation method be:Diethylene glycol monolaurate and polyoxypropylene mannitol dioleate are added in silane coupling agent,
And 15~25min is stirred in 40~60 DEG C, then 30~40min is kept the temperature, it then cools to room temperature up to surface conditioning agent.
7. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that the silane coupling agent
For the volume in Silane coupling agent KH550 or silane coupling agent KH560 any one, and the content of silane coupling agent be more than 98%.
8. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that shaken in the step S2
Water temperature when swinging in concussion instrument is 30~50 DEG C, amplitude 20mm, and rotating speed is 100~300r/min.
9. a kind of chemical treatment method on magnetic powder surface according to claim 1, which is characterized in that true in the step S2
The dry temperature of sky is 98~108 DEG C.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113233688A (en) * | 2021-04-29 | 2021-08-10 | 中国矿业大学(北京) | Method for treating mine water |
CN115231855A (en) * | 2022-07-13 | 2022-10-25 | 天津鑫路桥建设工程有限公司 | Magnetic powder modified asphalt and preparation process thereof |
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CN85107789A (en) * | 1985-10-23 | 1987-04-22 | 化学工业部第一胶片厂 | The chemical treatment method on magnetic surface |
US20130153088A1 (en) * | 2011-12-15 | 2013-06-20 | Vacuumschmelze Gmbh & Co. Kg | Method for producing a rare earth-based magnet |
CN105328200A (en) * | 2014-07-15 | 2016-02-17 | 昆山玛冀电子有限公司 | Atomization pelleting method for soft magnetic powder |
WO2016097568A1 (en) * | 2014-12-15 | 2016-06-23 | Universite Paul Sabatier - Toulouse Iii | Material consisting of friable micrometric aggregates comprising nanometric particles |
CN106915822A (en) * | 2017-02-21 | 2017-07-04 | 济南大学 | A kind of composite magnetic particle based on aluminium nickel cobalt and preparation method thereof |
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2018
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Patent Citations (5)
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CN85107789A (en) * | 1985-10-23 | 1987-04-22 | 化学工业部第一胶片厂 | The chemical treatment method on magnetic surface |
US20130153088A1 (en) * | 2011-12-15 | 2013-06-20 | Vacuumschmelze Gmbh & Co. Kg | Method for producing a rare earth-based magnet |
CN105328200A (en) * | 2014-07-15 | 2016-02-17 | 昆山玛冀电子有限公司 | Atomization pelleting method for soft magnetic powder |
WO2016097568A1 (en) * | 2014-12-15 | 2016-06-23 | Universite Paul Sabatier - Toulouse Iii | Material consisting of friable micrometric aggregates comprising nanometric particles |
CN106915822A (en) * | 2017-02-21 | 2017-07-04 | 济南大学 | A kind of composite magnetic particle based on aluminium nickel cobalt and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113233688A (en) * | 2021-04-29 | 2021-08-10 | 中国矿业大学(北京) | Method for treating mine water |
CN115231855A (en) * | 2022-07-13 | 2022-10-25 | 天津鑫路桥建设工程有限公司 | Magnetic powder modified asphalt and preparation process thereof |
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Application publication date: 20180724 |