CN108941604A - A kind of preparation method of novel simple block nanometer iron powder - Google Patents
A kind of preparation method of novel simple block nanometer iron powder Download PDFInfo
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- CN108941604A CN108941604A CN201810864351.5A CN201810864351A CN108941604A CN 108941604 A CN108941604 A CN 108941604A CN 201810864351 A CN201810864351 A CN 201810864351A CN 108941604 A CN108941604 A CN 108941604A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention discloses a kind of preparation method of novel simple block nanometer iron powder, include the following steps: to configure raw material, the raw material is that ferric nitrate and reducing agent are dissolved in the solution formed in deionized water, the mass ratio of the ferric nitrate and reducing agent: 10:3;Solid-state heating;By aspirating hole to vacuum warehouse internal air exhausting, the vacuum degree inside vacuum warehouse reaches 1.0 × 10-1 Pa;The circulatory system for opening the vacuum warehouse vacuumizes 20 ~ 40min to vacuum warehouse, and vacuum warehouse reaches capacity 6.6 × 10-2 of vacuum Pa;Inert gas is filled to vacuum warehouse;Process solid-state intermediary;Nanometer iron powder and the cooling of vacuum warehouse temperature reach 20 ~ 45 DEG C;Argon gas is filled to the vacuum warehouse, vacuum warehouse is made to restore atmospheric pressure;Vacuum warehouse is opened, the nanometer iron powder is discharged in discharge gate.The preparation method of the novel simple block nanometer iron powder, simple process can be effectively ensured nanometer iron powder and examine quality, and guarantee meets the requirement that the high-precision end such as electronics, communication, space flight, aviation uses.
Description
Technical field
The present invention relates to nanometer irony fabricating technology field more particularly to a kind of novel simple block nanometer iron powders
Preparation method.
Background technique
Nano material is the current and following material for most having development potentiality, due to its unique skin effect, bulk effect
And quantum size effect, so that the performances such as the electricity of material, mechanics, magnetics, optics produce surprising variation.Nano material
With quantum effect, small-size effect and skin effect, many distinctive physics, chemical property can be showed and therefore obtain material
The heat of the domain experts such as material is held in both hands.Metal nano material is an important component of nano material, and metal nano material will be golden
Belong to unique physicochemical properties organically to combine with the property of nano material, be widely used in electronics, communication,
The fields such as space flight, aviation, wide market.
The research and development of nano material is made a general survey of, it is not difficult to find out that, the popularization and application key of nano material is block nanometer material
The preparation of material, and the main target of Bulk Nanocrystalline Metals technology of preparing development is then that development process is simple, yield is applicable in greatly
Range is wide, can obtain example interface cleaning, the macro nanometer material preparation technology of pore-free gap.Its development trend is then development
The nanocrystalline technology of preparing of direct crystallization method.It is believed that with the continuous research and development of lumpy nanometer material preparation technology, not far
There will be the appearances of more nano materials, and generate huge social and economic benefits.
However, Nano metal powder, especially nanometer iron powder production technology are complicated in the prior art, the nanometer iron powder of production is pure
Degree is told somebody what one's real intentions are, and the use at the high-precision end such as the use of nanometer iron powder, especially electronics, communication, space flight, aviation is influenced.
It can be seen that nanometer iron powder production technology in the prior art exists, production technology is complicated, the quality of nanometer iron powder
It is poor, influence the defect of the subsequent usage of nanometer iron powder.
Summary of the invention
In view of this, nanometer iron powder can be effectively ensured and examine the main purpose of the present invention is to provide a kind of simple process
Quality is looked into, guarantees the preparation side for meeting the novel simple block nanometer iron powder that the high-precision end such as electronics, communication, space flight, aviation uses
Method.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of preparation method of novel simple block nanometer iron powder, includes the following steps:
S1, configuration raw material;The raw material is that ferric nitrate and reducing agent are dissolved in the solution formed in deionized water, the ferric nitrate and
The mass ratio of reducing agent: 10:6;
S2, solid-state heating;Raw material heating prepared by the S1, solution evaporation, concentration, decomposition obtain solid-state intermediary;
S3, vacuum warehouse is opened, vacuum is added to the vacuum warehouse inner cavity cleaning, and by the solid-state intermediary of step S2 preparation
Inside storehouse;
S4, the circuit connection and air-channel system for checking the vacuum warehouse;
S5, vacuum warehouse is closed, the vacuum by aspirating hole to 8 ~ 15min of the vacuum warehouse internal air exhausting, inside the vacuum warehouse
Degree reaches 1.0 × 10-1 Pa;
S6, the circulatory system for opening the vacuum warehouse vacuumize 20 ~ 40min to vacuum warehouse, and the vacuum warehouse reaches capacity vacuum
6.6×10-2 Pa;
S7, inert gas is filled to vacuum warehouse, the pressure of the vacuum warehouse is 0.2-0.6pa;
S8, capacitor power switch is connected, gives capacitor charging, process solid-state intermediary;
Solid-state intermediary described in S9, completion of processing shuts down 50min ~ 70min;
S10, nanometer iron powder and vacuum warehouse temperature reach 20 ~ 45 DEG C;
S11, inert gas is filled to the vacuum warehouse, vacuum warehouse is made to restore atmospheric pressure;
S12, vacuum warehouse is opened, the nanometer iron powder is discharged in discharge gate;
S13, nanometer iron powder classification is required to be collected into respectively seperated collection vessel;
S14, packaging screening;The nanometer iron powder gathered is screened to packaging inside packing case.
In a preferred embodiment, the inert gas is argon gas, and the purity of the argon gas is 99.999%.
In a preferred embodiment, in the step S7, the pressure of vacuum warehouse is 0.4pa.
In a preferred embodiment, in the step S8 ~ S10, the pressure of the vacuum warehouse is 0.5pa.
In a preferred embodiment, in the step S5, by the aspirating hole to pumping inside the vacuum warehouse
Gas 10min.
In a preferred embodiment, in the step S6, by the aspirating hole to pumping inside the vacuum warehouse
Gas 30min.
In a preferred embodiment, in the step S9, solid-state intermediary described in completion of processing shuts down 60min.
In a preferred embodiment, in the step S10, nanometer iron powder and vacuum warehouse temperature reach 20 DEG C.
The preparation method of novel simple block nanometer iron powder of the invention, has the following beneficial effects:
The preparation method of the novel simple block nanometer iron powder configures raw material;Solid-state heating;By aspirating hole to vacuum warehouse inside
Pumping;Inert gas is filled to vacuum warehouse;Process solid-state intermediary;Nanometer iron powder and the cooling of vacuum warehouse temperature reach 20 ~ 45 DEG C;
Argon gas is filled to the vacuum warehouse, vacuum warehouse is made to restore atmospheric pressure;Vacuum warehouse is opened, the Nanoscale Iron is discharged in discharge gate
Powder.Avoid that nanometer iron powder production technology in the prior art is complicated, nanometer iron powder it is second-rate, after influencing nanometer iron powder
The defect of continuous usage.Nanoscale Iron can be effectively ensured in the preparation method of the novel simple block nanometer iron powder, simple process
Powder examines quality, and guarantee meets the requirement that the high-precision end such as electronics, communication, space flight, aviation uses.
Specific embodiment
Make below with reference to preparation method of the embodiment of the present invention to novel simple block nanometer iron powder of the invention into one
Step detailed description.
A kind of preparation method of novel simple block nanometer iron powder, includes the following steps:
S1, raw material is configured by weighing;Raw material is that ferric nitrate and reducing agent are dissolved in the solution formed in deionized water, ferric nitrate and
The mass ratio of reducing agent: 10:6;The reducing agent is at least one of glycine, alanine, urea, citric acid.Ferric nitrate
Mass ratio between reducing agent can be 10:2 ~ 7, as long as can satisfy reduction effect, can also be produced according to production
The difference that product require, selects the reducing agent of various dose, to meet the nanometer iron powder for producing different requirements.Raw material is mixed it
Afterwards, it stirs, makes it completely dissolved, and be uniformly mixed.
S2, configured raw material is further processed, carries out solid-state heating;Raw material heating prepared by step S1, solution
Volatilization, is decomposed at concentration, and solid-state intermediary is obtained;Decomposable process discharges a large amount of gas, and chemistry reflection occurs.
S3, vacuum warehouse is opened, to vacuum warehouse inner cavity cleaning, avoids reducing product quality to impurity is increased in raw material;Again will
The solid-state intermediary of step S2 preparation is added inside vacuum warehouse.
S4, the circuit connection and air-channel system for checking vacuum warehouse;Guarantee that equipment smoothly can orderly work, protects
Demonstrate,prove producers' safety.
S5, vacuum warehouse is closed, by aspirating hole to vacuum warehouse 8 ~ 15min of internal air exhausting, the vacuum degree inside vacuum warehouse reaches
To 1.0 × 10-1 Pa;
S6, the circulatory system for opening the vacuum warehouse vacuumize 20 ~ 40min to vacuum warehouse, and the vacuum warehouse reaches capacity vacuum
6.6×10-2 Pa;Vacuum warehouse is vacuumized twice by step S5 and step S6, reaches higher vacuum requirement, reduces and takes out very
Empty difficulty, also further decreases the requirement to vacuum warehouse intensity.
S7, inert gas (protective gas) is filled to vacuum warehouse, the pressure of vacuum warehouse is 0.2-0.6pa;First provides pressure
Power, second pair of raw material protective effect guarantee that during the reaction, the foreign gas that reactant nearby enriches is fewer.
S8, capacitor power switch is connected, gives capacitor charging, process solid-state intermediary;By arc through, realize better
Meet chemistry reflection, guarantees the quality of product.
S9, completion of processing solid-state intermediary shut down 50min ~ 70min;It shuts down, by the circulation of outside air, to vacuum
Nanometer iron powder cooling inside storehouse and vacuum warehouse, reaches room temperature.Preferably, other refrigerating plants or portion can be passed through
Part is realized and quickly cools down to the nanometer iron powder inside vacuum warehouse and vacuum warehouse, product is avoided to aoxidize.
S10, nanometer iron powder and vacuum warehouse temperature reach 20 ~ 45 DEG C;It is substantially at the identical problem of room temperature, it preferably can be with
Lower than room temperature, the possibility that product is oxidized is further decreased.
S11, inert gas is filled to vacuum warehouse, vacuum warehouse is made to restore atmospheric pressure;It is filled by argon gas, guarantees vacuum warehouse
Internal pressure and ambient pressure balance, so that making opening vacuum warehouse, internal and external pressure balance guarantees the safety of equipment, Yi Jisheng
The safety of production personnel.
S12, vacuum warehouse is opened, nanometer iron powder (finished product) is discharged in discharge gate;
S13, nanometer iron powder classification is required to be collected into respectively seperated collection vessel;
S14, packaging screening;The nanometer iron powder gathered is screened to packaging inside packing case.
Preferably, inert gas is argon gas, and the purity of argon gas is 99.999%.The argon gas of high concentration may further be to anti-
Object protective effect is answered, and comparatively cost is relatively low for argon gas, the argon gas of high concentration is also easy to get.
It is obtained by many experiments, in the step s 7, the pressure of vacuum warehouse is 0.4pa.Both the quality of product can have been guaranteed.
Further, in step S8 ~ S10, the pressure of vacuum warehouse is 0.5pa.
Personnel's operation and control in order to facilitate processing, and the setting to automatically processing device, can select step S5
In, 10min is determined as to the vacuum warehouse internal air exhausting time by aspirating hole, can satisfy the requirement used, i.e. pressure is unlikely to
It is too big or too small.
In step S6, by aspirating hole to vacuum warehouse internal air exhausting 30min.
In step S9, solid-state intermediary described in completion of processing shuts down 60min.
In step S10, nanometer iron powder and vacuum warehouse temperature reach 20 DEG C.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (8)
1. a kind of preparation method of novel simple block nanometer iron powder, which comprises the steps of:
S1, configuration raw material;The raw material is that ferric nitrate and reducing agent are dissolved in the solution formed in deionized water, the ferric nitrate and
The mass ratio of reducing agent: 10:6;
S2, solid-state heating;Raw material heating prepared by the S1, solution evaporation, concentration, decomposition obtain solid-state intermediary;
S3, vacuum warehouse is opened, vacuum is added to the vacuum warehouse inner cavity cleaning, and by the solid-state intermediary of step S2 preparation
Inside storehouse;
S4, the circuit connection and air-channel system for checking the vacuum warehouse;
S5, vacuum warehouse is closed, the vacuum by aspirating hole to 8 ~ 15min of the vacuum warehouse internal air exhausting, inside the vacuum warehouse
Degree reaches 1.0 × 10-1 Pa;
S6, the circulatory system for opening the vacuum warehouse vacuumize 20 ~ 40min to vacuum warehouse, and the vacuum warehouse reaches capacity vacuum
6.6×10-2 Pa;
S7, inert gas is filled to vacuum warehouse, the pressure of the vacuum warehouse is 0.2-0.6pa;
S8, capacitor power switch is connected, gives capacitor charging, process solid-state intermediary;
Solid-state intermediary described in S9, completion of processing shuts down 50min ~ 70min;
S10, nanometer iron powder and vacuum warehouse temperature reach 20 ~ 45 DEG C;
S11, inert gas is filled to the vacuum warehouse, vacuum warehouse is made to restore atmospheric pressure;
S12, vacuum warehouse is opened, the nanometer iron powder is discharged in discharge gate;
S13, nanometer iron powder classification is required to be collected into respectively seperated collection vessel;
S14, packaging screening;The nanometer iron powder gathered is screened to packaging inside packing case.
2. the preparation method of novel simple block nanometer iron powder according to claim 1, which is characterized in that the indifferent gas
Body is argon gas, and the purity of the argon gas is 99.999%.
3. the preparation method of novel simple block nanometer iron powder according to claim 1, which is characterized in that the step S7
In, the pressure of vacuum warehouse is 0.4pa.
4. the preparation method of novel simple block nanometer iron powder according to claim 1, which is characterized in that the step S8
In ~ S10, the pressure of the vacuum warehouse is 0.5pa.
5. the preparation method of novel simple block nanometer iron powder according to claim 1, which is characterized in that the step S5
In, by the aspirating hole to the vacuum warehouse internal air exhausting 10min.
6. the preparation method of novel simple block nanometer iron powder according to claim 1, which is characterized in that the step S6
In, by the aspirating hole to the vacuum warehouse internal air exhausting 30min.
7. the preparation method of novel simple block nanometer iron powder according to claim 1, which is characterized in that the step S9
In, solid-state intermediary described in completion of processing shuts down 60min.
8. the preparation method of novel simple block nanometer iron powder according to claim 1, which is characterized in that the step
In S10, nanometer iron powder and vacuum warehouse temperature reach 20 DEG C.
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