CN1203431A - Method for making iron nitride magnetic fluid - Google Patents
Method for making iron nitride magnetic fluid Download PDFInfo
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- CN1203431A CN1203431A CN 98101595 CN98101595A CN1203431A CN 1203431 A CN1203431 A CN 1203431A CN 98101595 CN98101595 CN 98101595 CN 98101595 A CN98101595 A CN 98101595A CN 1203431 A CN1203431 A CN 1203431A
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Abstract
A process for preparing magnetic fluid of iron nitride uses iron carbonyl liquid and ammonia gas as raw materials and includes such technological steps as evaporating iron carbonyl liquid, passing the vapour along with carrying gas into a mixer, after mixing it with diluting gas and ammonia gas, introducing the mixure through perforated plate into reactor containing preloaded carrying liquid, and reaction of vapour of iron carbonyl on ammonia gas to generate magnetic iron nitride particles dispersed in carrying liquid to form iron nitride magnetic fluid that has higher saturated magnetization intensity.
Description
The invention relates to a metal magnetic material, in particular to a magnetic liquid of a metal matrix composite material. Magnetic liquid (magnetic liquid and magnetofluid for short) is a metastable sol system formed by highly dispersing nanometer-sized magnetic particles (single-domain magnetic particles) in oil-based liquid through a surfactant, and the surfactant and the oil-based liquid form a carrier liquid. Even under the action of external field force (such as gravity, centrifugal force and electromagnetic force), the magnetic particles and the carrier liquid do not separate and still move integrally. Under the condition of no external magnetic field, it does not show magnetism, and its magnetic hysteresis loop is an S-shaped curve passing through coordinate origin.
The saturation magnetization of the magnetic liquid depends on the magnetic properties of the magnetic particles and the volume percentage of the particles in the carrier liquid; and the fluid characteristics (such as vapor pressure, freezing point, viscosity and the like) of the oil-based fluid are mainly determined by the original characteristics of the oil-based fluid.
The metal (such as iron) magnetic liquid has high saturation magnetization and high initial magnetic permeability, but is easily oxidized in the atmospheric environment, and the magnetism is gradually reduced. In order to overcome the above disadvantages, magnetic liquids of metal-based compounds, such as iron nitride magnetic liquids, were developed internationally in the early nineties. The magnetic liquid is a new type of magnetic liquid, which has corrosion resistance obviously superior to that of metal type magnetic liquid, and the saturation magnetization can be improved by adopting a concentration method. Iron nitride magnetic liquids having high saturation magnetization have been prepared in japan. The high-performance iron nitride magnetic liquid has wide application prospect.
US5180512 provides a method for producing a ferromagnetic nitride liquid. The method takes carbonyl iron, ammonia gas, argon gas and oil as raw materials, a solution formed by the carbonyl iron and kerosene is put into a reactor, and polyamine surfactant is added into the solution. The specific process is that the reactor is heated to 90 ℃, the temperature is kept for 1 hour, then the temperature is raised to 185 ℃, the temperature is kept for 1 hour, and ammonia gas is input into the reactor during the whole heating period. The heating process is repeated for 3-6 times until all carbonyl iron in the kerosene is decomposed. Finally, high boiling point hydrocarbon oil is used to replace kerosene.
The method needs to be heated and cooled for many times, and has complex process and great operation difficulty. In addition, the method adds the raw materials into the reaction furnace together, and the purity of the product is difficult to control.
Chinese patent CN 1144967a discloses a method and apparatus for manufacturing metal magnetic liquid. The method adopts thermal decomposition method, firstly, the ferromagnetic metal is made into liquid carbonyl metal compound, and placed in a container, and evaporated to form carbonyl iron vapour, said vapour is carried into a mixer by carrier gas, and after dilution, it is fed into a decomposing furnace through a porous plate, and is thermally decomposed in the furnace to produce nano-grade metal particles, and then the nano-grade metal particles are dispersed in the carrier liquid to form the metal magnetic liquid. The device consists of a thermostatic bath, an evaporation container, a mixer, a porous plate, a thermal decomposition furnace and corresponding pipelines.
The manufacturing method provided by the patent can only produce metal type magnetic liquid. The range of use is limited and a magnetic liquid of a metal-based compound type, such as a ferromagnetic nitride liquid, cannot be produced.
The invention aims to provide a method for producing a ferro-magnetic fluid nitride, which is simple and can produce a metal-based compound type magnetic liquid.
The preparation method of the iron nitride magnetic fluid takes carbonyl iron liquid, ammonia gas and carrier gas (nitrogen, argon, hydrogen or mixed gas thereof) as raw materials, the carbonyl iron liquid is evaporated to form carbonyl iron vapor, the carbonyl iron vapor and the ammonia gas are mixed in a mixer and then enter a reaction furnace through a porous plate to carry out decomposition-synthesis reaction, and finally the iron nitride magnetic liquid is formed.
The method of the invention is implemented on a ferro-fluid nitride preparation device.
The present invention will now be described in detail with reference to the accompanying drawings.
FIG. 1 shows an apparatus for preparing a ferrofluid nitride according to the present invention.
In the figure, 1 is a regulating valve, 2 is a flow meter, 3 is an evaporator, 4 is a constant temperature bath, 6 is a heating insulation sleeve, 7 is a reaction furnace, 8 is a mixer, 9 is a porous plate, 10 is carrier liquid, 11 is a temperature display and control instrument, 12, 13 and 14 are pipelines, 15 is a tail gas discharge pipe, 16 is carbonyl iron liquid, 17 is a measurement and control line, and 18, 19 and 20 are input pipelines of carrier gas, diluent gas and ammonia gas respectively. The evaporator 3 is in the thermostatic bath 4; one end of the pipeline 12 extends into the carbonyl iron liquid 16, one end of the pipeline 13 is positioned above the liquid level of the carbonyl iron liquid, and the other end is communicated with the mixer 8; the porous plate 9 is positioned between the mixer 8 and the reaction furnace 7, and the porous plate 9 is a ventilating and oil-tight partition plate; the heating and heat-insulating sleeve 6 is positioned around the reaction furnace and has the functions of adjusting the reaction temperature and insulating heat.
The invention relates to a manufacturing method of a ferro-magnetic nitride fluid, which comprises the following specific process steps:
[1] evaporation of liquid iron carbonyls
Putting carbonyl iron liquid into an evaporation container 3 in a constant temperature bath 4, evaporating the carbonyl iron liquid, controlling the evaporation temperature to be 30-90 ℃, and conveying carbonyl iron vapor obtained by evaporation into a mixer 8 through a pipeline 13 by using carrier gas;
[2] dilution of carbonyl iron vapor
The mixed gas composed of the carrier gas and the carbonyl iron vapor input into the mixer 8 is mixed with the diluent gas input by the pipeline 19, and the carbonyl iron vapor is further diluted;
the carrier gas and the diluent gas can be any one or any two of nitrogen, argon and hydrogen.
[3] While the dilution gas is fed into the mixer 8, ammonia gas is fed into the mixer 8 through the pipe 20, and the ratio (volume ratio) of the dilution gas to the ammonia gas is: 1: 15-50;
[4] the carbonyl iron steam and ammonia gas are subjected to 'decomposition-synthesis' reaction in a reaction furnace 7
Before working, the carrier liquid composed of oil base liquid and surfactant is put into the reaction furnace 7 in advance, and heated to the temperature range of 150-245 ℃, and the mixed gas composed of carbonyl iron vapor, carrier gas, diluent gas and ammonia enters the reaction furnace 7 from the mixer 8 through the porous plate 9. The gas mixture foams the carrier liquid in the reaction furnace to form countless small bubbles with the diameter of about 1mm, each small bubble is a 'gas phase reactor', and carbonyl iron vapor and ammonia gas generate 'decomposition-synthesis' reaction in the bubbles, and the reaction formula is as follows:
the above reaction is almost instantaneously completed at the same time. Fe formed3N is a nanocrystal of Fe3N then enters the bubbleThe oil film around the wall is covered with carrier liquid, thus preventing the possibility of crystal growth. Fe in the carrier liquid with prolonged reaction time3The concentration of the N magnetic fine particles becomes higher and higher, and a practically useful iron nitride magnetic liquid having a high saturation magnetization can be obtained.
The oil base fluid in the carrier fluid can be any one of base oil, diffusion pump oil, white oil, ester oil and synthetic oil; the surfactant can be any one of octadecylamine, barium petroleum sulfonate, imine, magnesium stearate and sodium oleate.
Compared with the prior art, the invention has the following advantages:
(1) the process steps are simple, the process is easy to control, and the cost is low.
(2) The prepared magnetic fluid has high purity and good performance.
(3) The product can be directly used after being prepared without changing carrier liquid.
Examples
By adopting the method and the ferro-magnetic nitride fluid preparation device, four batches of ferro-magnetic nitride fluid are prepared by taking carbonyl iron liquid and ammonia gas as basic raw materials. The raw materials used are shown in Table 1, and the parameters of the preparation process, such as evaporation temperature, reaction temperature and time of "decomposition-synthesis", the ratio of carrier gas, diluent gas and ammonia gas, and the total flow rate thereof are shown in Table 2. The four batches of the prepared iron nitride magnetic fluid are subjected to centrifugal and external magnetic field tests, and test results prove that iron nitride magnetic particles and carrier liquid are still not separated, and the iron nitride magnetic particles and the carrier liquid move integrally in the test process. Four batches of ferrofluid were also sampled to measure the average particle size and saturation magnetization of the magnetic particles, and the results are shown in Table 3.
Table 1 raw materials used in the examples
| Batch number | Basic raw material | Oil-based fluid | Surfactant | Carrier gas | Dilution gas |
| 1 | Carbonyl iron liquid, Ammonia gas | Hydrocarbon oil | Octadecamine | Argon gas | Argon gas |
| 2 | Carbonyl iron liquid, Ammonia gas | Base oil | Barium sulfonate | Argon gas | Nitrogen gas |
| 3 | Carbonyl iron liquid, Ammonia gas | White oil | Imine(s) | Argon, hydrogen Mixed gas (es) | Argon and hydrogen mixture Gas mixture |
| 4 | Carbonyl iron liquid, Ammonia gas | Ester oil | Magnesium stearate | Hydrogen gas | Hydrogen gas |
TABLE 2 Process parameters of the examples
TABLE 3 characteristics of the ferrofluid nitrides obtained in the examples
| Batch number | Evaporation temperature ℃ | Decomposition synthesis reaction | Carrier gas flow Measurement of ml/min | Dilution gas and ammonia Ratio of qi to blood (volume ratio) | Dilution gas and ammonia Total flow of gas ml/min | |
| Temperature of | Time of day 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 |
| Batch number | Iron nitride particles Average particle size Å | Saturation magnetization (Gauss) |
| 1 | 180 | 700 |
| 2 | 150 | 623 |
| 3 | 120 | 667 |
| 4 | 100 | 553 |
Claims (1)
1. A method of manufacturing a nitrided ferrofluid comprising the steps of:
[1] evaporation of liquid iron carbonyls
Putting carbonyl iron liquid into an evaporation container (3) in a constant temperature tank (4) to evaporate the carbonyl iron liquid, controlling the evaporation temperature at 30-90 ℃, and sending carbonyl iron vapor obtained by evaporation into a mixer (8) through a pipeline (13) by using carrier gas;
[2] dilution of carbonyl iron vapor
The mixed gas composed of the carrier gas and the carbonyl iron vapor input into the mixer (8) is mixed with the diluent gas input by the pipeline (19), and the carbonyl iron vapor is further diluted;
[3] at the same time of inputting the diluent gas, inputting ammonia gas into the mixer (8) through a pipeline (20), wherein the proportion (volume ratio) of the diluent gas to the ammonia gas is as follows: 1: 15-50;
[4] mixed gas consisting of carrier gas, diluent gas, ammonia gas and carbonyl iron vapor enters a reaction furnace (7) through a mixer (8) through a porous plate (9) to react; a carrier liquid consisting of oil-based liquid and a surfactant is placed in the reaction furnace (7) in advance;
[5] the carbonyl iron steam and ammonia gas are subjected to decomposition-synthesis reaction
After entering a reaction furnace (7) from a mixer (8) through a porous plate (9), the mixed gas of carbonyl iron vapor, ammonia gas and the like and the carrier liquid which is preheated to the temperature of 150-:
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 |
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| 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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| CN1203431A true CN1203431A (en) | 1998-12-30 |
| CN1056460C CN1056460C (en) | 2000-09-13 |
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| CN98101595A Expired - Fee Related CN1056460C (en) | 1998-04-29 | 1998-04-29 | Method for making iron nitride magnetic fluid |
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Cited By (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 |
| CN102963872A (en) * | 2011-09-02 | 2013-03-13 | 浩华科技实业有限公司 | Device and method for preparing nitrided iron micro powders |
| CN106694905A (en) * | 2017-03-03 | 2017-05-24 | 中国工程物理研究院激光聚变研究中心 | Preparation method and preparation devices for nanometer 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049996C (en) * | 1995-09-04 | 2000-03-01 | 冶金工业部钢铁研究总院 | Manufacture method and device for metal magnetic liquid |
-
1998
- 1998-04-29 CN CN98101595A patent/CN1056460C/en not_active Expired - Fee Related
Cited By (5)
| 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 |
| CN102963872A (en) * | 2011-09-02 | 2013-03-13 | 浩华科技实业有限公司 | Device and method for preparing nitrided iron micro powders |
| 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 |
| CN106694905A (en) * | 2017-03-03 | 2017-05-24 | 中国工程物理研究院激光聚变研究中心 | Preparation method and preparation devices for nanometer 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 |
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| Publication number | Publication date |
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| CN1056460C (en) | 2000-09-13 |
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