CN112556505A - Energy-containing semiconductor bridge based on Al/PVDF (aluminum/polyvinylidene fluoride) ink and preparation method thereof - Google Patents
Energy-containing semiconductor bridge based on Al/PVDF (aluminum/polyvinylidene fluoride) ink and preparation method thereof Download PDFInfo
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- CN112556505A CN112556505A CN202011314352.6A CN202011314352A CN112556505A CN 112556505 A CN112556505 A CN 112556505A CN 202011314352 A CN202011314352 A CN 202011314352A CN 112556505 A CN112556505 A CN 112556505A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F42—AMMUNITION; BLASTING
- F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
- F42B3/00—Blasting cartridges, i.e. case and explosive
- F42B3/10—Initiators therefor
- F42B3/12—Bridge initiators
- F42B3/13—Bridge initiators with semiconductive bridge
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention discloses an energy-containing semiconductor bridge based on Al/PVDF printing ink and a preparation method thereof. The method comprises the steps of dispersing nano aluminum powder in N-methyl pyrrolidone solution of PVDF to obtain Al/PVDF ink, dripping the Al/PVDF ink on the surface of a semiconductor bridge chip in a micro-pen direct writing mode, drying and then obtaining the Al/PVDF energetic film on the semiconductor bridge chip. The Al/PVDF ink has the advantages of high reaction heat release, high combustion flame propagation speed and the like, and the energetic semiconductor bridge based on the Al/PVDF ink has high ignition output capability and good safety and can realize gap ignition.
Description
Technical Field
The invention belongs to the technical field of semiconductor bridges, and relates to an energy-containing semiconductor bridge based on Al/PVDF (aluminum/polyvinylidene fluoride) ink and a preparation method thereof.
Background
The semiconductor bridge is a bridge film type transducer element based on a semiconductor film or a metal-semiconductor film which generates heat or plasma energy under external electric energy stimulation, and is one of the most important initiating explosive device transducer elements developed through microelectronic integration technology in the field of semiconductor devices in recent years. The trigger circuit has the advantages of low trigger energy, high instantaneous property, high safety, high reliability, capability of being combined with a digital logic circuit and the like. Although the semiconductor bridge meets the requirements of safety and reliability, the semiconductor bridge has the condition of low ignition output capability due to small bridge area, and can only ignite sensitive initiating explosive such as lead stigmatisate and the like at present and can not meet the requirement of insensitive ignition.
How to effectively improve the ignition output capability of the semiconductor bridge under the condition of ensuring the safety of the semiconductor bridge is a difficult problem to be solved urgently by semiconductor bridge ignition products. Therefore, researchers develop researches on the energy-containing semiconductor bridge, energy-containing films with certain thickness are integrated on the surface of the semiconductor bridge through various film preparation technologies, when external energy such as heat energy, electric energy or laser radiation is excited, the energy-containing films can generate self-sustaining combustion reaction to emit a large amount of heat, and simultaneously, glowing solid products are generated to be sprayed out along with sparks generated when the semiconductor bridge is ignited, so that the ignition output capacity of the semiconductor bridge is effectively improved. The common energetic film mainly comprises a metal alloying film and a metal/oxide film, and the main film components comprise Al/Ni, Al/Ru, Al/CuO and Al/MoO3And the like.
In the preparation process of the energy-containing film, nano aluminum powder is a very important raw material, but the particle surface of the nano aluminum powder can be oxidized to form a layer of compact Al2O3And a passivation layer. The existence of the passivation layer obviously reduces the content of active aluminum in the aluminum powder so as to reduce the energy density of the nano aluminum powder, and simultaneously, the passivation layer (mainly Al) is used for reducing the energy density of the nano aluminum powder2O3) High melting temperature of (A) will result inThe ignition temperature of the nano aluminum powder is increased, the burning rate is reduced, so that the energy is not completely released during the reaction, the reaction process is influenced to a certain extent, the reaction performance of the finally prepared energy-containing film cannot meet the actual requirement, and the ignition output performance of a semiconductor bridge integrated with the energy-containing film is influenced.
Disclosure of Invention
The invention aims to provide an energy-containing semiconductor bridge based on aluminum/polyvinylidene fluoride (Al/PVDF) ink and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows:
the preparation method of the energy-containing semiconductor bridge based on the Al/PVDF printing ink integrates the Al/PVDF printing ink on the surface of a semiconductor bridge chip by adopting a micro straight writing technology to form an Al/PVDF film, and comprises the following steps:
step 1, dissolving PVDF in N-methyl pyrrolidone at 70-80 ℃ to prepare a PVDF solution with the concentration of 0.1-2.0 mol/L;
step 2, according to the mass ratio of 1: 1-1.5: 1 of the nano aluminum powder to the PVDF, firstly, ultrasonic mixing is adopted, and then, the nano aluminum powder is uniformly dispersed into the PVDF solution in a magnetic mechanical stirring mode to obtain Al/PVDF ink;
and 3, integrating Al/PVDF ink on the semiconductor bridge chip in a micro-pen direct writing mode, drying the semiconductor bridge, sequentially and circularly integrating and drying, drying the semiconductor bridge after the ink is completely integrated, and finally integrating an Al/PVDF film on the surface of the semiconductor bridge chip to obtain the energy-containing semiconductor bridge based on the Al/PVDF ink.
Preferably, in the step 2, the activity of the nano aluminum powder is 60-75%.
Preferably, in the step 2, the ultrasonic mixing time is 1-3 hours, and the magnetic mechanical stirring time is 12-36 hours.
Preferably, in the step 3, the micro-straight writing times are 2-5 times, the drying temperature after each integration is 50 ℃, and the drying time is 20-40 min; and after all the printing ink is integrated, the drying temperature is 50 ℃, and the drying time is 2-6 h.
Compared with the prior art, the invention has the remarkable advantages that:
(1) PVDF can be used as a passivation layer (mainly Al) on the surface of nano aluminum powder2O3) Solid-solid phase pre-ignition reaction to generate AlF3The influence of the surface passivation layer on the reaction performance of the nano aluminum powder is overcome. At the same time, the aluminum powder particles are fluorinated to generate AlF3The released energy is 55.7KJ/g which is far higher than the energy (31KJ/g) released when the aluminum powder particles are oxidized, so that the Al/PVDF film has the advantages of high reaction heat release, high combustion flame propagation speed and the like, and the ignition output capability of the semiconductor bridge can be greatly improved by the integrated Al/PVDF film.
(2) The poor thermal conductivity of PVDF enables the Al/PVDF film to be insensitive, and the safety of the semiconductor bridge can be guaranteed while the ignition output capacity of the semiconductor bridge is effectively improved. Experiments are carried out according to the requirements of GJB5309.14-2004 'initiating explosive device experiment method: 1A1W5min non-firing experiment', and the energy-containing semiconductor bridge based on the Al/PVDF ink is proved to pass a safe current experiment.
Drawings
FIG. 1 is a flow chart of the preparation of an Al/PVDF ink-based energetic semiconductor bridge of the present invention.
FIG. 2 is an SEM representation of the Al/PVDF film of example 1.
FIG. 3 is an image of the moment of ignition of an energetic semiconductor bridge based on Al/PVDF ink under 40V pulsed voltage excitation in example 1.
FIG. 4 shows the energetic semiconductor bridge ignition B/KNO based on Al/PVDF ink under 40V pulsed voltage excitation in example 13The image of the moment of ignition.
FIG. 5 is an image of the moment of ignition of an energetic semiconductor bridge based on Al/PVDF ink under 40V pulsed voltage excitation in example 2.
FIG. 6 shows the energetic semiconductor bridge ignition B/KNO based on Al/PVDF ink under 40V pulsed voltage excitation in example 23The image of the moment of ignition.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific examples, which are provided for illustration only and are not intended to limit the invention in any way.
Example 1
The preparation method of the energy-containing semiconductor bridge based on the Al/PVDF printing ink comprises the following specific steps:
step 1, weighing 0.24g of PVDF, and dissolving in 3ml of N-methylpyrrolidone at 70 ℃ to prepare a PVDF solution;
step 2, weighing 0.24g of nano aluminum powder (the activity is measured to be 65%) and adding the nano aluminum powder into the PVDF solution, ultrasonically mixing for 1h, and then magnetically and mechanically stirring for 24h to obtain Al/PVDF ink;
and 3, integrating the Al/PVDF printing ink on the semiconductor bridge chip by adopting a micro-pen direct writing mode, and then placing the semiconductor bridge chip in an oven to dry for 30min at the temperature of 50 ℃. And (3) circularly writing for 3 times according to the steps, and after the printing ink is completely integrated, placing the printing ink in a drying oven to be dried for 4 hours at 50 ℃ to obtain the energy-containing semiconductor bridge with the Al/PVDF film attached to the surface of the semiconductor bridge chip.
The microscopic morphology of the prepared Al/PVDF film is characterized by a scanning electron microscope, and the result is shown in FIG. 2, which shows that Al and PVDF are uniformly distributed on a solvent carrier net structure in the Al/PVDF film, and the Al and PVDF prepared by the method are uniformly dispersed and well contacted.
By means of an energy storage discharge initiator, an ignition experiment is carried out on the energy-containing semiconductor bridge based on the Al/PVDF printing ink under the condition of 40V pulse voltage excitation ignition, an ignition instant image is collected by a camera, and the result is shown in figure 3, which shows that the energy-containing semiconductor bridge based on the Al/PVDF printing ink reliably ignites, the flame burns violently, and the fire is bright under the condition of 40V pulse voltage excitation.
By means of gap ignition, B/KNO3The interval between the ignition powder and the prepared energy-containing semiconductor bridge is set to be 3mm, the energy-containing semiconductor bridge based on the Al/PVDF ink is subjected to a gap ignition experiment under the condition of 40V pulse voltage excitation ignition, an ignition instant image is collected by a camera, and the result is shown in figure 4, which shows that the energy-containing semiconductor bridge based on the Al/PVDF ink can reliably ignite B/KNO at the 3mm gap under the 40V pulse voltage excitation3The ignition powder has strong ignition capability and has gap ignition capability.
The energy-containing semiconductor bridge based on the Al/PVDF ink is subjected to a safe current test by means of an intelligent detonator electrical parameter tester, and the result shows that the energy-containing semiconductor bridge based on the Al/PVDF ink passes the requirements of GJB5309.14-2004 'experimental method for initiating explosive devices, 1A1W5min non-firing experiment'.
Example 2
The preparation method of the energy-containing semiconductor bridge based on the Al/PVDF printing ink comprises the following specific steps:
step 1, weighing 0.24g of PVDF, and dissolving in 3ml of N-methylpyrrolidone at 70 ℃ to prepare a PVDF solution;
step 2, weighing 0.36g of nano aluminum powder (the activity is measured to be 65%) and adding the nano aluminum powder into the PVDF solution, ultrasonically mixing for 1h, and then magnetically and mechanically stirring for 24h to obtain Al/PVDF ink;
and 3, integrating the Al/PVDF printing ink on the semiconductor bridge chip by adopting a micro-pen direct writing mode, and then placing the semiconductor bridge chip in an oven to dry for 30min at the temperature of 50 ℃. And (3) circularly writing for 3 times according to the steps, and after the printing ink is completely integrated, placing the printing ink in a drying oven to be dried for 4 hours at 50 ℃ to obtain the energy-containing semiconductor bridge with the Al/PVDF film attached to the surface of the semiconductor bridge chip.
By means of an energy storage discharge initiator, an ignition experiment is carried out on the energy-containing semiconductor bridge based on the Al/PVDF printing ink under the condition of 40V pulse voltage excitation ignition, an ignition instant image is collected by a camera, and the result is shown in figure 5, which shows that the energy-containing semiconductor bridge based on the Al/PVDF printing ink reliably ignites under the condition of 40V pulse voltage excitation, the flame combustion is obvious, and the fire light is bright.
By means of gap ignition, B/KNO3The interval between the ignition powder and the prepared energy-containing semiconductor bridge is set to be 3mm, the energy-containing semiconductor bridge based on the Al/PVDF ink is subjected to a gap ignition experiment under the condition of 40V pulse voltage excitation ignition, an ignition instant image is collected by a camera, and the result is shown in figure 5, which shows that the energy-containing semiconductor bridge based on the Al/PVDF ink can reliably ignite B/KNO at the 3mm gap under the 40V pulse voltage excitation3The ignition powder has strong ignition capability and has gap ignition capability.
The energy-containing semiconductor bridge based on the Al/PVDF ink is subjected to a safe current test by means of an intelligent detonator electrical parameter tester, and the result shows that the energy-containing semiconductor bridge based on the Al/PVDF ink passes the requirements of GJB5309.14-2004 'experimental method for initiating explosive devices, 1A1W5min non-firing experiment'.
Comparative example 1
This comparative example is essentially the same as example 1, except that the mass ratio of the nano aluminum powder to PVDF is 0.5: 1.
By means of an energy storage discharge exploder, ignition experiments are carried out on the energy-containing semiconductor bridge based on the Al/PVDF printing ink under the condition of 40V pulse voltage excitation ignition, and the result shows that the energy-containing semiconductor bridge based on the Al/PVDF printing ink does not ignite under the condition of 40V pulse voltage excitation.
By means of gap ignition, B/KNO3The interval between the ignition powder and the prepared energy-containing semiconductor bridge is set to be 3mm, and the energy-containing semiconductor bridge based on the Al/PVDF ink is subjected to a gap ignition experiment under the condition of 40V pulse voltage excitation and ignition, and the result shows that under the 40V pulse voltage excitation, the energy-containing semiconductor bridge based on the Al/PVDF ink does not ignite and cannot ignite B/KNO at the 3mm gap3An ignition charge.
The safe current test is carried out on the energy-containing semiconductor bridge based on the Al/PVDF ink by means of an intelligent detonator electrical parameter tester, and the result shows that the resistance of the energy-containing semiconductor bridge based on the Al/PVDF ink is obviously changed before and after the test, and the resistance cannot pass the requirements of GJB5309.14-2004 'experimental method for initiating explosive devices, namely 1A1W5min non-firing experiment'.
Comparative example 2
This comparative example is essentially the same as example 1, except that the mass ratio of the nano aluminum powder to PVDF is 0.75: 1.
By means of an energy storage discharge exploder, ignition experiments are carried out on the energy-containing semiconductor bridge based on the Al/PVDF printing ink under the condition of 40V pulse voltage excitation ignition, and the result shows that the energy-containing semiconductor bridge based on the Al/PVDF printing ink does not ignite under the condition of 40V pulse voltage excitation.
By means of gap ignition, B/KNO3The interval between the ignition powder and the prepared energy-containing semiconductor bridge is set to be 3mm, and the energy-containing semiconductor bridge based on the Al/PVDF ink is subjected to a gap ignition experiment under the condition of 40V pulse voltage excitation ignition, and the result shows that the gap ignition experiment is carried out at 40V pulseUnder the excitation of impulse voltage, the energy-containing semiconductor bridge based on the Al/PVDF printing ink does not ignite and can not ignite B/KNO at the 3mm gap3Ignition powder
The safe current test is carried out on the energy-containing semiconductor bridge based on the Al/PVDF ink by means of an intelligent detonator electrical parameter tester, and the result shows that the resistance of the energy-containing semiconductor bridge based on the Al/PVDF ink is obviously changed before and after the test, and the resistance cannot pass the requirements of GJB5309.14-2004 'experimental method for initiating explosive devices, namely 1A1W5min non-firing experiment'.
Claims (6)
1. The preparation method of the energy-containing semiconductor bridge based on the Al/PVDF printing ink is characterized by comprising the following steps:
step 1, dissolving PVDF in N-methyl pyrrolidone at 70-80 ℃ to prepare a PVDF solution with the concentration of 0.1-2.0 mol/L;
step 2, according to the mass ratio of 1: 1-1.5: 1 of the nano aluminum powder to the PVDF, firstly, ultrasonic mixing is adopted, and then, the nano aluminum powder is uniformly dispersed into the PVDF solution in a magnetic mechanical stirring mode to obtain Al/PVDF ink;
and 3, integrating Al/PVDF ink on the semiconductor bridge chip in a micro-pen direct writing mode, drying the semiconductor bridge, sequentially and circularly integrating and drying, drying the semiconductor bridge after the ink is completely integrated, and finally integrating an Al/PVDF film on the surface of the semiconductor bridge chip to obtain the energy-containing semiconductor bridge based on the Al/PVDF ink.
2. The preparation method according to claim 1, wherein in the step 2, the activity of the nano aluminum powder is 60-75%.
3. The preparation method according to claim 1, wherein in the step 2, the ultrasonic mixing time is 1-3 h, and the magnetic mechanical stirring time is 12-36 h.
4. The production method according to claim 1, wherein in step 3, the number of times of the fine straight writing is 2 to 5 times.
5. The preparation method according to claim 1, wherein in the step 3, the drying temperature after each integration is 50 ℃ and the drying time is 20-40 min.
6. The preparation method according to claim 1, wherein in the step 3, the drying temperature is 50 ℃ and the drying time is 2-6 h after the ink is completely integrated.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115043690A (en) * | 2022-05-09 | 2022-09-13 | 南京理工大学 | Preparation method of silver ignition bridge based on ink-jet direct writing |
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Application publication date: 20210326 |