CN1056460C - Method for making iron nitride magnetic fluid - Google Patents
Method for making iron nitride magnetic fluid Download PDFInfo
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- CN1056460C CN1056460C CN98101595A CN98101595A CN1056460C CN 1056460 C CN1056460 C CN 1056460C CN 98101595 A CN98101595 A CN 98101595A CN 98101595 A CN98101595 A CN 98101595A CN 1056460 C CN1056460 C CN 1056460C
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- carbonyl iron
- liquid
- ammonia
- fluid
- carrier gas
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Abstract
The present invention relates to the field of a metallic magnetic material and is mainly suitable for the preparation of metal based compound magnetic fluid. The method of the present invention takes ironpentacarbonyl liquid and ammonia gas as raw materials. The process of the present invention comprises the steps: firstly, the ironpentacarbonyl liquid is evaporated; the steam enters a mixer along with carrier gas and then enters a reaction furnace via a perforated plate after being mixed with diluent gas and the ammonia gas; carrier liquid has been added to the reaction furnace beforehand; in the furnace, the ironpentacarbonyl steam and the ammonia gas react to generate magnetic particle iron nitride, and the iron nitride is dispersed in the carrier liquid to form iron nitride magnetic fluid. The magnetic fluid has higher saturation magnetization.
Description
The present invention relates to metallicl magnetic material, particularly the magnetic liquid of metal-base composites.
Magnetic liquid (being called for short magnetic liquid, magnetic fluid again) is that a kind of magnetic particle by nano-scale (single domain magnetic grain) passes through interfacial agent high degree of dispersion formed metastable state sol system in oil-base fluid, and interfacial agent and oil-base fluid have constituted carrier fluid.Even under the effect of outfield force (as gravity, centrifugal force, electromagnetic force), magnetic particle does not separate with carrier fluid yet, still do mass motion.Do not having under the external magnetic field effect, itself does not show magnetic, and its magnetic hysteresis loop is a S type curve by origin of coordinate.
The saturation magnetization of magnetic liquid depends on the magnetic characteristic of magnetic particle and particulate shared percentage by volume in carrier fluid; And its fluid behaviour (as vapour pressure, solidifying point, viscosity etc.) depends primarily on the primary characteristic of oil-base fluid.
The saturation magnetization height of metal (as iron) magnetic liquid, initial permeability is big, but oxidation easily takes place in it under atmospheric environment, and magnetic descends gradually.Give to produce and use makes troubles and inconvenience, in order to overcome above-mentioned shortcoming, the early 1990s, succeeded in developing the magnetic liquid of Metal Substrate compound in the world, as magnetic liquid of nitriding iron.This is a kind of novel magnetic liquid, and its corrosion resistance obviously is better than the metal mold magnetic liquid, and can adopt concentrated way to improve saturation magnetization.Japan has produced the magnetic liquid of nitriding iron with high saturation and magnetic intensity.High performance magnetic liquid of nitriding iron will have broad application prospects.
U.S. Pat 5180512 provides a kind of manufacture method of magnetic liquid of nitriding iron.This method is a raw material with carbonyl iron, ammonia, argon gas and fluid, and the solution of carbonyl iron and kerosene formation is put into reactor, has also added polyamine class interfacial agent in this liquid.Its concrete technology is that reactor is heated to 90 ℃, is incubated 1 hour, rises to 185 ℃ again, is incubated 1 hour again, between the whole period of heating, imports ammonia in reactor.Above-mentioned heating process will be successively 3-6 time repeatedly, and the carbonyl iron in kerosene all has been decomposed.Also to come substituting coal oil at last with the high boiling hydrocarbon wet goods.
This method needs through the cooling that repeatedly heats up, complex process, and operation easier is big.In addition, this method is with raw material-and add in the reacting furnace, and the degree of purity of product is restive.
Chinese patent CN1144967A discloses a kind of manufacture method and device of metal magnetic liquid.This method adopts thermal decomposition method, at first ferromagnetic metal is made liquid carbonyl metal compound, and placed container, make it evaporation, form the carbonyl iron steam, this steam is brought in the blender by carrier gas, after dilution, enters dore furnace by porous plate in the lump, in stove, carry out thermal decomposition, generate the nano level metal particulate, and be scattered in the carrier fluid, form metal magnetic liquid.Its device is made up of thermostat, container for evaporation, blender, porous plate, thermal decomposition furnace and corresponding pipeline.
The manufacture method that this patent provided can only production metal mold magnetic liquid.The scope of application is restricted, and magnetic liquid that can not production Metal Substrate compound type is as magnetic liquid of nitriding iron.
The object of the present invention is to provide a kind of method simple, the manufacture method of the iron nitride magnetic fluid of energy production Metal Substrate compound type magnetic liquid.
The manufacture method of iron nitride magnetic fluid of the present invention is a raw material with carbonyl iron liquid, ammonia and carrier gas (nitrogen, argon gas, hydrogen or its mist), carbonyl iron liquid forms the carbonyl iron steam after evaporating, in blender with after ammonia mixes, pass through porous plate in the lump, enter in the reacting furnace, carry out " decomposing-synthetic " reaction, finally form magnetic liquid of nitriding iron.
Method of the present invention is implemented on the iron nitride magnetic fluid preparation facilities.
Now in conjunction with the accompanying drawings, the present invention is elaborated.
Accompanying drawing 1 is iron nitride magnetic fluid preparation facilities of the present invention.
Among the figure, 1 is control valve, and 2 is flowmeter, 3 is evaporimeter, and 4 is thermostat, and 6 is the heat tracing cover, 7 is reacting furnace, and 8 is blender, and 9 is porous plate, 10 is carrier fluid, and 11 are temperature demonstration and controller, and 12,13,14 is pipeline, 15 is exhaust emission tube, 16 is carbonyl iron liquid, and 17 for measuring and control circuit, and 18,19,20 are respectively the input channel of carrier gas, carrier gas and ammonia. Evaporimeter 3 is in the thermostat 4; One of pipeline 12 is stretched among the carbonyl iron liquid 16, a top that is in the carbonyl iron liquid levels of pipeline 13, and the other end communicates with blender 8; Porous plate 9 is between blender 8 and the reacting furnace 7, and porous plate 9 is ventilative oil-resisting dividing plate; Heat tracing cover 6 be in reacting furnace around, have the reaction temperature of adjustment and insulation effect.
The manufacture method of iron nitride magnetic fluid of the present invention, its concrete technology step is as follows:
[1] evaporation of carbonyl iron liquid
Carbonyl iron liquid is placed container for evaporation 3 in the thermostat 4, make it evaporation, evaporating temperature is controlled at 30-90 ℃, and the carbonyl iron steam that will evaporate gained with carrier gas is sent in the blender 8 by pipeline 13;
[2] dilution of carbonyl iron steam
Carrier gas in the input mixer 8 and carbonyl iron steam mix with the diluent gas of being imported by pipeline 19, and the carbonyl iron steam further dilutes;
Above-mentioned described carrier gas and carrier gas can be in nitrogen, argon gas, the hydrogen any or any two gaseous mixture.
[3] in the input carrier gas, by pipeline 20, import ammonia in blender 8, the ratio of carrier gas and ammonia (volume ratio) is: 1: (15-50);
[4] mist of being made up of carrier gas, carrier gas, ammonia and carbonyl iron steam passes through porous plate 9, is entered in the reacting furnace 7 by blender 8, reacts, and has placed the carrier fluid of being made up of oil-base fluid and interfacial agent in the reacting furnace in advance;
[5] carbonyl iron steam and ammonia carry out " decomposing-synthetic " reaction in reacting furnace 7
Before the work, in advance the carrier fluid of oil-base fluid and interfacial agent composition is put into reacting furnace 7, and be heated in the 150-245 ℃ of temperature range described mist, after entering reacting furnace 7, carry out " decomposing-synthetic " reaction with the carrier fluid of heating, gaseous mixture makes the carrier fluid foaming in the reacting furnace, forms the minute bubbles of the about 1mm of countless diameters, each minute bubbles all is one " Gas-phase reactor ", in bubble, " decomposing-synthetic " reaction takes place in carbonyl iron steam and ammonia, and its reaction equation is as follows:
Above-mentioned reaction is almost finished in moment simultaneously.Formed Fe
3N is a nanocrystal, this nanocrystal Fe
3N enters in the oil film around the walls immediately, is cladded by carrier fluid, thereby has prevented the possibility of grain growth.Along with the prolongation in reaction time, Fe in the carrier fluid
3The concentration of N magnetic particle is more and more higher, thereby can obtain to have the magnetic liquid of nitriding iron of the high saturation and magnetic intensity of practical value.
Oil-base fluid in the above-mentioned carrier fluid can be in base oil, diffusion pump oil, white oil, ester class oil, the artificial oil any; Interfacial agent can adopt in octadecylamine, barium mahogany sulfonate, imines, dolomol, the enuatrol any.
Compared with prior art, the present invention has following advantage:
(1) processing step is simple, and technical process is easy to control, and cost is low.
(2) prepared magnetic fluid high purity, performance is good.
(3) after product is produced, can directly use, need not change carrier fluid.
Embodiment
Adopting method of the present invention and iron nitride magnetic fluid preparation facilities, is base stock with carbonyl iron liquid and ammonia, has prepared four batches of magnetic liquid of nitriding iron.The raw material that is adopted is as shown in table 1, and ratio and the total flow thereof of producing parameter in the process such as evaporating temperature, " decompose--synthetic " reaction temperature and time, carrier gas, carrier gas and ammonia are as shown in table 2.Carry out centrifugal and the externally-applied magnetic field test to four batches of iron nitride magnetic fluids being produced, result of the test proof iron nitride magnetic particulate does not still separate with carrier fluid, and both do mass motion always in the process of the test.Go back the magnetic particle particle mean size and the saturation magnetization of four batches of iron nitride magnetic fluids of sampling and measuring simultaneously, its result lists table 3 in.
Table 1 embodiment is raw materials used
| Lot number | Base stock | Oil-base fluid | Interfacial agent | Carrier gas | Carrier gas |
| 1 | Carbonyl iron liquid, ammonia | Hydrocarbon ils | Octadecylamine | Argon gas | Argon gas |
| 2 | Carbonyl iron liquid, ammonia | Base oil | Barium sulfonate | Argon gas | Nitrogen |
| 3 | Carbonyl iron liquid, ammonia | White oil | Imines | Argon, hydrogen gaseous mixture | Argon, hydrogen gaseous mixture |
| 4 | Carbonyl iron liquid, ammonia | Ester class oil | Dolomol | Hydrogen | Hydrogen |
The technological parameter of table 2 embodiment
The characteristic of the iron nitride magnetic fluid that table 3 embodiment is produced
| Lot number | Evaporating temperature ℃ | Decompose synthetic reaction | Carrier gas flux ml/min | The ratio (volume ratio) of carrier gas and ammonia | Carrier gas and ammonia total flow ml/min | |
| Temperature ℃ | Time hr | |||||
| 1 | 56 | 230 | 54 | 100 | 1∶45 | 900 |
| 2 | 45 | 230 | 48 | 120 | 1∶30 | 700 |
| 3 | 30 | 200 | 48 | 170 | 1∶25 | 500 |
| 4 | 30 | 190 | 48 | 200 | 1∶20 | 300 |
| Lot number | Nitrided iron particulate particle mean size | Saturation magnetization (Gauss) |
| 1 | 180 | 700 |
| 2 | 150 | 623 |
| 3 | 120 | 667 |
| 4 | 100 | 553 |
Claims (1)
1, a kind of manufacture method of iron nitride magnetic fluid comprises:
[1] carbonyl iron evaporation of liquid
Carbonyl iron liquid is placed the interior container for evaporation (3) of thermostat (4), make it evaporation, evaporating temperature is controlled at 30-90 ℃, will evaporate gained carbonyl iron steam with carrier gas and send in the blender (8) by pipeline (13);
[2] dilution of carbonyl iron steam
Carrier gas in the input mixer (8) and carbonyl iron steam mix with the diluent gas of being imported by pipeline (19), and the carbonyl iron steam is further diluted,
It is characterized in that:
[1] in the input diluent gas, by pipeline (20), input ammonia in blender (8), the ratio of carrier gas and ammonia (volume ratio) is: 1: (15-50);
[2] mist of being made up of carrier gas, carrier gas, ammonia and carbonyl iron steam passes through porous plate (9), is entered in the reacting furnace (7) by blender (8), reacts; Reacting furnace has been placed the carrier fluid of being made up of oil-base fluid and interfacial agent in (7) in advance;
[3] carbonyl iron steam and ammonia carry out " decomposing-synthetic " reaction in reacting furnace (7)
After described mist enters reacting furnace (7) by porous plate (9) by blender (8), carry out " decomposing-synthetic " reaction with the carrier fluid that is heated to 150-245 ℃ of temperature in advance, generate iron nitride magnetic fluid, its reaction equation is as follows:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101595A CN1056460C (en) | 1998-04-29 | 1998-04-29 | Method for making iron nitride magnetic fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101595A CN1056460C (en) | 1998-04-29 | 1998-04-29 | Method for making iron nitride magnetic fluid |
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| Publication Number | Publication Date |
|---|---|
| CN1203431A CN1203431A (en) | 1998-12-30 |
| CN1056460C true CN1056460C (en) | 2000-09-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98101595A Expired - Fee Related CN1056460C (en) | 1998-04-29 | 1998-04-29 | Method for making iron nitride magnetic fluid |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358061C (en) * | 2005-04-14 | 2007-12-26 | 钢铁研究总院 | Method for preparing magnetic liquid of nitriding iron by using concentrating agent of low volatilization point |
| CN102963872B (en) * | 2011-09-02 | 2014-11-26 | 浩华科技实业有限公司 | Device and method for preparing nitrided iron micro powders |
| CN106694905B (en) * | 2017-03-03 | 2019-09-03 | 中国工程物理研究院激光聚变研究中心 | The preparation method and preparation facilities of a kind of nanometer of beryllium powder |
| CN113059182A (en) * | 2020-01-02 | 2021-07-02 | 吉林卓创新材料有限公司 | Preparation method of carbonyl iron powder special for magnetic grinding fluid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1144967A (en) * | 1995-09-04 | 1997-03-12 | 冶金工业部钢铁研究总院 | Manufacture method and device for metal magnetic liquid |
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1998
- 1998-04-29 CN CN98101595A patent/CN1056460C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1144967A (en) * | 1995-09-04 | 1997-03-12 | 冶金工业部钢铁研究总院 | Manufacture method and device for metal magnetic liquid |
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|---|---|
| CN1203431A (en) | 1998-12-30 |
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