CN109678630A - The preparation method of Al/NiO sheet thermite - Google Patents
The preparation method of Al/NiO sheet thermite Download PDFInfo
- Publication number
- CN109678630A CN109678630A CN201910021708.8A CN201910021708A CN109678630A CN 109678630 A CN109678630 A CN 109678630A CN 201910021708 A CN201910021708 A CN 201910021708A CN 109678630 A CN109678630 A CN 109678630A
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- Prior art keywords
- nio
- sheet
- substrate
- thermite
- presoma
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Classifications
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
Abstract
The preparation method of Al/NiO sheet thermite, comprising: the peelable metallic substrates of sheet are provided；Configure hydrothermal synthesis reaction liquid；Hydrothermal synthesis reaction is executed to obtain presoma in substrate；Presoma is roasted so that NiO lamella is formed on the substrate；The finally magnetron sputtering nanometer aluminium film again on NiO lamella, to obtain sheet Al/NiO Energetic Nanomaterials laminated film.Thermite of the invention stores, is easy to carry, and production cost is low, and environmental-friendly, combustion heat release is had excellent performance.
Description
Technical field
The present invention relates to a kind of preparation methods of Energetic Nanomaterials laminated film.
Background technique
Only aluminium powder and metal oxide is simply mixed in traditional thermite, so aluminothermy surface reaction rate is slower, point
Fiery temperature is higher, and actual thermal discharge is also very low, is difficult to meet the needs of the special industries high requirement such as military affairs.It is more existing
Although laboratory thermite preparation method improves to some extent at many aspects, in the mass transfer rate of thermit reaction, technological design, ring
Border friendly, ease of use and industrialized production etc. are still unsatisfactory.
Summary of the invention
The purpose of the present invention is to provide the more excellent thermites of performance.
According to the first aspect of the invention, a kind of preparation method of Al/NiO sheet thermite is provided, comprising:
Sheet metal substrate is provided；
Nickel sulfate and sodium hydroxide are mixed to form mixed liquor with molar ratio 1:2 or so；
It the use of the pH value that sulfuric acid adjusts mixed liquor is 5-9；
Mixed liquor dislocation after adjusting pH value is entered in reaction kettle；
It is put into substrate in a kettle again；
Make temperature of reaction kettle keep 150~260 DEG C, reaction 12~for 24 hours, thus in substrate attachment formed (light green color) before
Drive body；
The substrate for being attached with presoma is taken out, and presoma is cleaned by ultrasonic respectively using distilled water and ethyl alcohol；
To after cleaning presoma carry out calcination process NiO lamella is formed on the substrate, wherein maturing temperature be 300~
400 DEG C, calcining time 2h；
Then the NiO lamella formed in substrate is cooled to room temperature again；
The finally magnetron sputtering nanometer aluminium film again on NiO lamella, so that it is compound to obtain sheet Al/NiO Energetic Nanomaterials
Film.
It according to the method for the present invention, can also include: to be carried out to gained sheet Al/NiO Energetic Nanomaterials laminated film
Vacuum drying cooling.Later, can further include: from gained sheet Al/NiO Energetic Nanomaterials laminated film removal or
Stripping metal substrate.
It according to the method for the present invention, can also include: to be formed by mixed liquor in nickel sulfate and sodium hydroxide to be added, Isosorbide-5-Nitrae-
Butynediols and polyethylene glycol (PEG), wherein the molar ratio of Isosorbide-5-Nitrae-butynediols and PEG are 1:1 or so, Isosorbide-5-Nitrae-butynediols and
The molar ratio of nickel sulfate is 1:2000 or so.In the present invention, Isosorbide-5-Nitrae-butynediols helps to improve consistency and brightness, poly- second
Glycol then passes through the generation for improving the electrification situation realization sheet NiO on surface.
In the present invention, it is preferred to use PEG2000.
According to the present invention, magnetron sputtering parameter is preferred are as follows: back bias voltage 1.6 × 103V, interpolar is away from 0.07m, protective gas (argon
Gas) pressure 0.70Pa；Sputtering Plating times are 0.2~0.5h.
According to the present invention, metallic substrates can be Ti piece, Cu piece, stainless steel substrates or Ni piece, it is preferable to use Ni piece.
According to the second aspect of the invention, a kind of thermite is provided, is prepared by the above method.
By the present invention in that being simplified the collection work of presoma with metallic substrates and being facilitated subsequent processing and storage
It deposits.
Sheet metal substrate of the invention is further preferably further provided with geosutures, to form the suitable piece of required size
Area, consequently facilitating subsequent stripping metal substrate.In addition, as needed, can only remove (such as by executing letter along geosutures
Single breaks disconnected movement) required amount of section, to facilitate the storage and carrying of remaining thermite.
The present invention also has at least the following advantages:
Al/NiO sheet thermite Energetic Nanomaterials laminated film surface prepared by the present invention is evenly distributed, and substantially mentions
The contact area and uniformity coefficient for having risen aluminium powder and oxide, there's almost no agglomeration；
Al/NiO sheet thermite Energetic Nanomaterials laminated film exothermicity and combustibility prepared by the present invention
It is all good；
Operation of the present invention is simple, and preparation cost is cheap, and rate of film build is fast, is very suitable to industrial production；And
Present invention process is simple, environmental-friendly, has in industrial mass manufacture application and has great advantage.
Detailed description of the invention
Fig. 1 be according to the present invention provided by metallic substrates schematic diagrames；
Fig. 2 (a) and Fig. 2 (b) be respectively Al/NiO sheet thermite prepared according to the present invention scanning electron microscope (SEM) photograph and
Transmission electron microscope picture；
Fig. 3 is the DSC exotherm figure of Al/NiO sheet thermite prepared according to the present invention；And
Fig. 4 is the combustion flame figure of Al/NiO sheet thermite prepared according to the present invention.
Specific embodiment
The present invention is further illustrated below by embodiment.It should be appreciated by those skilled in the art that following embodiment is
In order to better understand and realize the present invention, it is not intended to restrict the invention.
As shown in Figure 1, present invention firstly provides the sheet substrate 10 of suitable size, such as nickel sheet.In substrate 10 setting or
Geosutures 11 and 12 are formed with, in order to subsequent strip operation.
The present invention configures hydrothermal synthesis reaction liquid as follows: nickel sulfate and sodium hydroxide being mixed to form with molar ratio 1:2 mixed
Liquid is closed, Isosorbide-5-Nitrae-butynediols and polyethylene glycol (PEG) is then added, wherein the molar ratio of Isosorbide-5-Nitrae-butynediols and PEG are 1:1,
The molar ratio of 1,4- butynediols and nickel sulfate is 1:2000；Reuse the pH value that sulfuric acid suitably adjusts mixed liquor.
Next will enter in hydrothermal synthesis reaction kettle (not specifically illustrated) with the reaction solution or mixed liquor dislocation that postpone, and
It is also put into substrate 10 in a kettle.Hydrothermal temperature remains 150~260 DEG C, and the reaction time is 12~for 24 hours, until
Attachment forms light green color presoma in substrate 10.
The substrate 10 for being attached with presoma is then taken out, and ultrasound is carried out clearly to presoma respectively using distilled water and ethyl alcohol
It washes.
Next calcination process is carried out to presoma to form NiO lamella on the substrate 10, maturing temperature is 300~700
DEG C, calcining time 2h.
Then the NiO lamella formed in substrate 10 is cooled to room temperature again.Rapid cooling is executed, such as is at least dropped per minute
50 DEG C of temperature, it will significantly reduce the binding force of thermite material and substrate 10 to be very beneficial for the subsequent removing of substrate 10.
Next the magnetron sputtering nanometer aluminium film again on NiO lamella, so that it is multiple to obtain sheet Al/NiO Energetic Nanomaterials
Close film.Magnetron sputtering parameter are as follows: back bias voltage 1.6 × 103V, interpolar is away from 0.07m, protective gas (argon gas) pressure 0.70Pa；It splashes
Penetrating Plating times is 0.2~0.5h.
Then vacuum drying cooling is carried out to gained sheet Al/NiO Energetic Nanomaterials laminated film.It later, can be with
From the removal of gained sheet Al/NiO Energetic Nanomaterials laminated film or stripping group bottom 10.For example, being got rid of along geosutures 11 and 12
Upper right a quarter shown in FIG. 1, and the substrate adhered to thereon is removed.
The present invention uses field emission scanning electron microscope (FESEM), differential scanning calorimeter (DSC), and high-speed camera etc. is to multiple
It closes film product and carries out surface topography and performance study analysis and characterization.
Embodiment 1
PEG uses PEG2000；Hydrothermal temperature remains 160 DEG C, and reaction time 12h, pH are adjusted to 7；Roasting temperature
350 DEG C of degree；Sputtering Plating times are 0.2h.
Using field emission scanning electron microscope (FESEM), differential scanning calorimeter (DSC), high-speed camera etc. is to laminated film
Product carries out surface topography and performance study is analyzed and characterized.Fig. 2 (a) and Fig. 2 (b) is the Al/ according to prepared by embodiment 1 respectively
The scanning electron microscope (SEM) photograph and transmission electron microscope picture of NiO sheet thermite；Fig. 3 is corresponding DSC exotherm figure, and thermal discharge is up to
1.5MJ Kg-1；Fig. 4 is then the combustion flame figure of the thermite.
Comparative example 2
The other the same as in Example 1, surfactant use PEG1000 instead, compare embodiment 1, the NiO being prepared is irregular
Shape and uneven, cannot achieve the later period preparation for the novel sheet thermite Al/NiO being evenly distributed.
Comparative example 3
The other the same as in Example 1, pH are adjusted to 5.Compared to embodiment 1, prepared Al/NiO sheet thermite thickness is slightly
It reduces, the thermal discharge of the sheet thermite is declined slightly about 1.43MJ Kg-1。
Comparative example 4
The other the same as in Example 1, hydrothermal temperature remain 140 DEG C.Compared to embodiment 1, prepared Al/NiO sheet
Thermite uniformity is poor, and heat release is obstructed, at this point, the thermal discharge of the sheet thermite is greatly reduced, Exotherm Time also occur compared with
Big delay.
Comparative example 5
The other the same as in Example 1, maturing temperature are promoted to 450 DEG C.Compared to embodiment 1, the thermal discharge of the sheet thermite is about
It is the 85% of 1 sample of example, in addition, phenomenon of bursting apart occurs in prepared Al/NiO sheet thermite, structure is unstable, is unfavorable for reality
Border uses.
Comparative example 6
The other the same as in Example 1, magnetron sputtering time halve.Compared to embodiment 1, the sheet thermite is living due to component reaction
Property substance metering than having relatively large deviation with the molar ratio of practical thermit reaction, therefore in sample NiO occur it is biggish it is remaining with
Waste, causes the energy fan-out capability of sample to greatly reduce, about the 45% of 1 sample of example.
As described above, the present invention uses in peelable substrate, recombinant magnetron sputtering is received after hydrothermal synthesis NiO presoma
Rice aluminium film, to obtain the sheet Al/NiO Energetic Nanomaterials laminated film haveing excellent performance.
Claims (6)
1. a kind of preparation method of Al/NiO sheet thermite, comprising:
Sheet metal substrate is provided；
Nickel sulfate and sodium hydroxide are mixed to form mixed liquor with molar ratio 1:2 or so；
It the use of the pH value that sulfuric acid adjusts mixed liquor is 5-9；
Mixed liquor dislocation after adjusting pH value is entered in reaction kettle；
It is put into substrate in a kettle again；
Make temperature of reaction kettle keep 150~260 DEG C, reaction 12~for 24 hours, thus in substrate attachment form presoma；
The substrate for being attached with presoma is taken out, and presoma is cleaned by ultrasonic respectively using distilled water and ethyl alcohol；
Calcination process is carried out so that NiO lamella is formed on the substrate to the presoma after cleaning, wherein maturing temperature is 300~400
DEG C, calcining time 2h；
Then the NiO lamella formed in substrate is cooled to room temperature again；
The finally magnetron sputtering nanometer aluminium film again on NiO lamella, to obtain sheet Al/NiO Energetic Nanomaterials laminated film.
2. the method according to claim 1, further includes: carry out vacuum to gained sheet Al/NiO Energetic Nanomaterials laminated film
Dry cooling.
3. method according to claim 2, further includes: remove or shell from gained sheet Al/NiO Energetic Nanomaterials laminated film
From metallic substrates.
4. the method according to claim 1, further includes: be formed by mixed liquor in nickel sulfate and sodium hydroxide and Isosorbide-5-Nitrae-butine is added
Two pure and mild polyethylene glycol (PEG), wherein the molar ratio of Isosorbide-5-Nitrae-butynediols and PEG are 1:1 or so, Isosorbide-5-Nitrae-butynediols and sulfuric acid
The molar ratio of nickel is 1:2000 or so.
5. method according to claim 4, wherein PEG is PEG2000.
6. the method according to claim 1, wherein metallic substrates are Ti piece, Cu piece, stainless steel substrates or Ni piece.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910021708.8A CN109678630B (en) | 2019-01-10 | 2019-01-10 | Preparation method of Al/NiO flaky thermite |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910021708.8A CN109678630B (en) | 2019-01-10 | 2019-01-10 | Preparation method of Al/NiO flaky thermite |
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| CN109678630A true CN109678630A (en) | 2019-04-26 |
| CN109678630B CN109678630B (en) | 2020-11-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357758A (en) * | 2019-08-08 | 2019-10-22 | 哈尔滨工业大学 | A kind of mesh structural porous NiO/Al Energetic Nanomaterials and preparation method thereof |
| CN110790618A (en) * | 2019-11-01 | 2020-02-14 | 南京理工大学 | Method for removing residual sulfur on surface of propellant powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101657553A (en) * | 2007-02-14 | 2010-02-24 | 表面处理技术公司 | The heat deposition of active metal oxide/aluminium lamination and the aluminide of dispersion-strengthened prepared therefrom |
| US20150101719A1 (en) * | 2013-10-10 | 2015-04-16 | Battelle Energy Alliance, Llc | Energetic materials and methods of tailoring electrostatic discharge sensitivity of energetic materials |
| CN105016935A (en) * | 2014-01-29 | 2015-11-04 | 香港城市大学 | Structure of energetic materials and the method for preparing thereof |
-
2019
- 2019-01-10 CN CN201910021708.8A patent/CN109678630B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101657553A (en) * | 2007-02-14 | 2010-02-24 | 表面处理技术公司 | The heat deposition of active metal oxide/aluminium lamination and the aluminide of dispersion-strengthened prepared therefrom |
| US20150101719A1 (en) * | 2013-10-10 | 2015-04-16 | Battelle Energy Alliance, Llc | Energetic materials and methods of tailoring electrostatic discharge sensitivity of energetic materials |
| CN105016935A (en) * | 2014-01-29 | 2015-11-04 | 香港城市大学 | Structure of energetic materials and the method for preparing thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357758A (en) * | 2019-08-08 | 2019-10-22 | 哈尔滨工业大学 | A kind of mesh structural porous NiO/Al Energetic Nanomaterials and preparation method thereof |
| CN110357758B (en) * | 2019-08-08 | 2021-07-27 | 哈尔滨工业大学 | Reticular porous NiO/Al nano energetic material and preparation method thereof |
| CN110790618A (en) * | 2019-11-01 | 2020-02-14 | 南京理工大学 | Method for removing residual sulfur on surface of propellant powder |
| CN110790618B (en) * | 2019-11-01 | 2020-12-08 | 南京理工大学 | Method for removing residual sulfur on surface of propellant powder |
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| CN109678630B (en) | 2020-11-10 |
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