CN103011243A - Preparation method of nano metal oxide and reaction device for preparing nano metal oxide - Google Patents
Preparation method of nano metal oxide and reaction device for preparing nano metal oxide Download PDFInfo
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- CN103011243A CN103011243A CN2012105264952A CN201210526495A CN103011243A CN 103011243 A CN103011243 A CN 103011243A CN 2012105264952 A CN2012105264952 A CN 2012105264952A CN 201210526495 A CN201210526495 A CN 201210526495A CN 103011243 A CN103011243 A CN 103011243A
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Abstract
The invention discloses a reaction device for preparing nano metal oxide and a preparation method of nano metal oxide. The reaction device comprises an explosion-proof tank body and a base which are in threaded fit with each other. The preparation method comprises the following steps: decomposing raw materials fast by utilizing instant high temperature and high pressure generated during explosion; and aggregating and crystallizing to form the nano material. The technology is a new research direction for the combination of the explosion mechanics and the materialogy. As the process is simple, and the raw materials are low in price and high in availability, industrialized production can be realized. No dispersant is used during the preparation process, so that hard aggregation among powder is eliminated. The obtained powder is uniform in particle size and narrow in distribution range. The detonation parameter, namely detonation pressure, can be tested accurately; and parameters such as the yield and the crystal form of nano metal oxide can be controlled by adjusting the detonation pressure.
Description
Technical field
The invention belongs to technical field of nano material, relate in particular to a kind of nano-metal-oxide preparation method and reaction unit of preparing.
Background technology
Detonation Process refers to utilize TRANSIENT HIGH TEMPERATURE and the high pressure of oxygen negative explosive blast generation; starting material are decomposed rapidly; then assemble crystallization and form the technology of nano material; it is the recent studies on direction of mechanics of explosion and materialogy combination; and technique is simple, effectively alleviates the pollution to environment, realizes easily mass-producing; be the green technology of preparation nano-powder, have good economic benefit and social benefit.Agglomeration Mechanism is conciliate to the mechanism of action and the blast impulse of nano materials in research explosive reaction field to the nano material hard aggregation analysis.The mechanism of action of explosive field be on the one hand to explode the gas that produces and High Temperature High Pressure field for the synthetic of nanoparticle and mutually transformation material and the energy are provided, oxygen negative explosive deposits in nanoparticle surface at the class gaseous state free carbon atom that explosion time produces on the other hand, the performance space steric effect is organized growth and the reunion of nanoparticle.
This method is a kind of cheapness, be easy to control processing parameter, near the synthetic method of gas phase.As a kind of brand-new synthetic technology, it relies on simple to operate, with low cost, is suitable for synthetic multiple simple substance, oxide compound and composite oxides, and characteristics applied widely have been subject to investigator's broad research.From detonation synthetic technology itself, can solve the problem of cheapness, pollution-free, a large amount of synthesis of nano oxide compound, nanometer double oxide.Detonation is synthetic not to need extra energy consumption, and detonation product generates N2 by chemical trim mode, and H2O and CO2 etc. realizes the purpose of environmental contamination reduction.Simultaneously detonation synthetic nanoparticle is actually and generates fast in the gas of high pressure high-density state, and expands with follow-up detonation gas one superhigh speed, is easy to prepare preferably nanoparticle of dispersiveness.Simultaneously, density, medicament proportioning by adjusting explosive, the means such as sensitizing agent of adding can realize the control to detonation parameter, and then the yardstick of the production technique of control nano-powder and nano-powder, crystal formation and composition composition, realize that the manual control of synthesis of nano powder and selectivity are synthetic.In view of conventional synthetic method in preparation during nano-oxide, the synthetic technology complexity is loaded down with trivial details, processing condition are restive, the shortcoming that yields poorly and Detonation Process are in superiority and the novelty of preparation nano-powder material, theory and practice experience and modern detonation theory achievement in research in conjunction with detonation synthesizing nano diamond, nano-graphite etc., Detonation Process prepares the research of nano oxide powder can not only enrich its preparation method, and can also promote to a certain extent the research of mechanism of detonation reaction to the correlative study of detonation product.Along with the fast development of other blast with researchs such as detonation phenomena such as shock compaction, explosive sintering, impact phase transformation, impact polarization and impact magnetization, will certainly promote the great development of detonation synthetic technology.The research of simultaneously, detonation nano materials also can provide certain theoretical and experiment to support to further improving detonation theory and the fine sight mechanics of explosion of development and the subject crossing such as chemistry, physics and materialogy conversely.
Summary of the invention
Of the present invention design emphatically one the blast synthesis reactor, adopting the solid mixt explosive is presoma, the different detonation parameter of control in the building-up process, such as the kind of explosive, detonation property, ratio, charging means etc. in raw material, record simultaneously detonation parameter, presoma proportioning and the experiment parameters such as form and detonation product, set up explosive property, form detonation parameter etc. to the size of synthetic nano alumina particles, the relation between the physical and chemical performance.
The embodiment of the invention is achieved in that a kind of reaction unit for preparing nano-metal-oxide, and described device comprises: an explosion-proof tank body (3) and a base (9), adopt thread fit between them; One of them explosion-proof tank body (3) is provided with relief hole (2), after detonation is finished, can make things convenient for pressure release and take off explosion-proof tank body (3); Four interfaces that are evenly distributed (10) are arranged on one of them base (9), be used for connecting oscilloscope, constant current source and pressure transmitter; Also have four electrodes (7) at base (9), material is brass, linked together by wire and interface (10), beaten four holes that are evenly distributed at base, good and sound interface (10) and electrode (7) seal with insulation paste.A pressure block (8) also on base, is used for fixing a pressure transmitter (6) and a powder column (5) and a detonator (4).
Further, an explosion-proof tank body (3) and a base (9) adopt treated stainless material, and a pressure release screw (1) employing is high pressure resistant, the screw of high temperature.
Further, four electrodes (7), material is brass; Four interfaces that are evenly distributed (10), they adopt insulation paste to seal after directly being connected by wire.
Further, a pressure block (8) adopts the tool steel material of high-temperature calcination, cooling process.
Further, a pressure transmitter (6) is selected copper-manganese sensor high temperature resistant, high pressure.
Further, a powder column (5) adopts explosive and the precursor mixture of location pressing method compacting.
Further, a detonator (4) adopts the industrial detonator of electric initiating.
Another purpose of the embodiment of the invention is to provide a kind of preparation method of nano-metal-oxide, and this preparation method comprises:
A certain proportion of explosive and metal oxide precursor are pressed into the mixing powder column of certain density according to location pressing method;
Soldered sensor and make to trigger probe, the adhesion powder column be connected detonator;
Connect oscilloscope and constant current source, use the constant current source primer detonator;
Record detonation pressure related data;
The cleaning blasting pot is collected detonation product, and cleaning impurity filters, the processing such as calcining, the gained solid product is carried out characterization research, to determine the parameters such as its pattern, crystalline structure.
Innovation of the present invention:
(1) TRANSIENT HIGH TEMPERATURE and the high pressure that produce with blast decompose rapidly starting material, and then assemble crystallization and form the technology of nano material, be the recent studies on direction of mechanics of explosion and materialogy combination.
(2) technique is simple, and raw material is cheap and easy to get, is expected to realize suitability for industrialized production.
(3) in preparation engineering, do not use dispersion agent, eliminated the hard aggregation between the powder.
(4) diameter of particle of gained is even, narrow distribution range.
(5) detonation parameter-detonation pressure can be accurately tested, the parameters such as yield, crystal formation of nano metal thing can be controlled by adjusting the detonation pressure size.
Description of drawings
Fig. 1 is the structural representation of the reaction unit of the preparation nano-metal-oxide that provides of the embodiment of the invention;
Fig. 2 is the schema that the reaction unit of the preparation nano-metal-oxide that provides of the embodiment of the invention is specifically participated in reaction.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
As shown in Figure 1, a kind of reaction unit for preparing nano-metal-oxide, described device comprises:
An explosion-proof tank body (3) and a base (9) adopt thread fit between them.
One of them explosion-proof tank body (3) is provided with relief hole (2), after detonation is finished, can make things convenient for pressure release and take off explosion-proof tank body (3).
Four Q9 interfaces (10) that are evenly distributed are arranged on one of them base (9), be used for connecting oscilloscope, constant current source and pressure transmitter; Also have four electrodes (7) at base (9), material is brass, linked together by wire and Q9 interface (10), beaten four holes that are evenly distributed at base, good and sound Q9 interface (10) and electrode (7) seal with insulation paste.A pressure block (8) also on base, is used for fixing a pressure transmitter (6) and a powder column (5) and a detonator (4).
A kind of reaction unit for preparing nano-metal-oxide, described device characteristic comprises:
An explosion-proof tank body (3) and a base (9) adopt the stainless material through special processing,
A pressure release screw (1) employing is high pressure resistant, the screw of high temperature;
Four electrodes (7), material is brass; Four Q9 interfaces (10) that are evenly distributed, they adopt insulation paste to seal after directly being connected by wire.
A pressure block (8) adopts the tool steel material of high-temperature calcination, cooling process.
A pressure transmitter (6) is selected copper-manganese sensor high temperature resistant, high pressure.
A powder column (5) adopts explosive and the precursor mixture of location pressing method compacting.
A detonator (4) adopts the industrial detonator of electric initiating.
As shown in Figure 2, reaction process is as follows:
(1) a certain proportion of explosive and metal oxide precursor are pressed into the mixing powder column of certain density according to location pressing method;
(2) soldered sensor and make to trigger probe, the adhesion powder column be connected detonator;
(3) connect oscilloscope and constant current source, use the constant current source primer detonator;
(4) record detonation pressure related data;
(5) the cleaning blasting pot is collected detonation product, and cleaning impurity filters, the processing such as calcining, the gained solid product is carried out characterization research, to determine the parameters such as its pattern, crystalline structure.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a reaction unit for preparing nano-metal-oxide is characterized in that, described device comprises: an explosion-proof tank body (3) and a base (9), adopt thread fit between them; One of them explosion-proof tank body (3) is provided with relief hole (2), after detonation is finished, can make things convenient for pressure release and take off explosion-proof tank body (3); Four interfaces that are evenly distributed (10) are arranged on one of them base (9), be used for connecting oscilloscope, constant current source and pressure transmitter;
Also have four electrodes (7) at base (9), material is brass, linked together by wire and interface (10), beaten four holes that are evenly distributed at base, good and sound interface (10) and electrode (7) seal with insulation paste; A pressure block (8) also on base, is used for fixing a pressure transmitter (6) and a powder column (5) and a detonator (4).
2. reaction unit as claimed in claim 1 is characterized in that, an explosion-proof tank body (3) and a base (9) adopt treated stainless material, and a pressure release screw (1) employing is high pressure resistant, the screw of high temperature.
3. reaction unit as claimed in claim 1 is characterized in that, four electrodes (7), and material is brass; Four interfaces that are evenly distributed (10), they adopt insulation paste to seal after directly being connected by wire.
4. reaction unit as claimed in claim 1 is characterized in that, a pressure block (8) adopts the tool steel material of high-temperature calcination, cooling process.
5. reaction unit as claimed in claim 1 is characterized in that, a pressure transmitter (6) is selected copper-manganese sensor high temperature resistant, high pressure.
6. reaction unit as claimed in claim 1 is characterized in that, a powder column (5) adopts explosive and the precursor mixture of location pressing method compacting.
7. reaction unit as claimed in claim 1 is characterized in that, a detonator (4) adopts the industrial detonator of electric initiating.
8. the preparation method of a nano-metal-oxide is characterized in that, this preparation method comprises:
A certain proportion of explosive and metal oxide precursor are pressed into the mixing powder column of certain density according to location pressing method;
Soldered sensor and make to trigger probe, the adhesion powder column be connected detonator;
Connect oscilloscope and constant current source, use the constant current source primer detonator;
Record detonation pressure related data;
The cleaning blasting pot is collected detonation product, and cleaning impurity filters, the processing such as calcining, the gained solid product is carried out characterization research, to determine the parameters such as its pattern, crystalline structure.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271402A (en) * | 2015-11-25 | 2016-01-27 | 西南科技大学 | Preparation method of zirconate gadolinium powder containing pyrochlore phase |
| CN107052331A (en) * | 2017-06-14 | 2017-08-18 | 南京理工大学 | Can pressure release type explosive sintering nanometer aluminium bar device and method |
| CN107824124A (en) * | 2017-11-13 | 2018-03-23 | 河南大学 | A kind of nano material preparation facilities and method |
| CN111380910A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Device for testing critical explosion temperature of explosive substance solution |
| CN111380911A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Device and method for testing critical explosion temperature of explosive substance solution |
| CN111380909A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Critical explosion temperature testing container for explosive material solution |
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| CN1382520A (en) * | 2002-02-01 | 2002-12-04 | 深圳市金刚源新材料发展有限公司 | Detonation process and equipment for synthesizing nano diamond |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271402A (en) * | 2015-11-25 | 2016-01-27 | 西南科技大学 | Preparation method of zirconate gadolinium powder containing pyrochlore phase |
| CN107052331A (en) * | 2017-06-14 | 2017-08-18 | 南京理工大学 | Can pressure release type explosive sintering nanometer aluminium bar device and method |
| CN107052331B (en) * | 2017-06-14 | 2020-04-10 | 南京理工大学 | Device and method for explosion sintering of nano aluminum bar capable of releasing pressure |
| CN107824124A (en) * | 2017-11-13 | 2018-03-23 | 河南大学 | A kind of nano material preparation facilities and method |
| CN111380910A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Device for testing critical explosion temperature of explosive substance solution |
| CN111380911A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Device and method for testing critical explosion temperature of explosive substance solution |
| CN111380909A (en) * | 2020-05-07 | 2020-07-07 | 中北大学 | Critical explosion temperature testing container for explosive material solution |
| CN111380911B (en) * | 2020-05-07 | 2022-09-16 | 中北大学 | Device and method for testing critical explosion temperature of explosive substance solution |
| CN111380909B (en) * | 2020-05-07 | 2023-03-31 | 中北大学 | Critical explosion temperature testing container for explosive material solution |
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Application publication date: 20130403 |