CN104529504A - Method for preparing micron-scale porous ceramic microspheres and electronic injection solution and device - Google Patents
Method for preparing micron-scale porous ceramic microspheres and electronic injection solution and device Download PDFInfo
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Abstract
The invention discloses a method for preparing micron-scale porous ceramic microspheres and an electronic injection solution and a device. The preparation method comprises the following steps: preparing an electronic injection solution, adjusting the power voltage to 15-20kV and the drive pressure to 0.1-0.6MPa, filling a receiving tank with water, absolute ethyl alcohol or mixture of water and absolute ethyl alcohol, performing electrostatic spraying and obtaining microsphere greens in a collecting tank; and filtering the microsphere greens with a Buchner funnel, drying for 1.5-3 hours at 80+/-5 DEG C, and sintering at high temperature to obtain the micron-scale porous ceramic microspheres. According to the method for preparing micron-scale porous ceramic microspheres disclosed by the invention, an electrostatic spraying method is adopted, the process is simple, the equipment is simple, automatic production can be realized at normal temperature, the electrostatically sprayed microspheres are uniformly dispersed without agglomeration, and the electrostatic spraying conditions can be controlled so as to accurately adjust the particle size and porosity of the microspheres; the electrostatic spraying can be performed simultaneously by adopting multiple electrostatic spraying needle cylinders and needles, and the working efficiency is high; and the preparation cost is low, little environmental pollution is caused, and the method is easy to popularize and use.
Description
Technical field
The invention belongs to materials science field, more specifically, the present invention relates to a kind of method utilizing electrostatic Spraying technique to prepare micrometer level porous ceramic microsphere and the EFI solution used and device.
Background technology
Stupalith has the advantages such as hardness is high, wear resistance good, solidity to corrosion is good, good insulating, is widely used in fields such as machinery, material, chemical industry, electric power, military affairs.Micron-size spherical ceramic particle can as the reinforcement material of matrix material or coating, and for improving the performance of body material, as wear resistance, solidity to corrosion, hardness, resistance to chemical corrosion, weathering resistance etc., application prospect is boundless.It can overcome the anisotropy of the irregular reinforcement materials such as needle-like, threadiness, sheet, reduces wedge angle position and produces stress concentration, thus improve matrix strength and plasticity.
The method preparing micro-ceramic microballoon at present mainly contains the precipitator method, polymerization-inducing colloidal aggregation method, sol-gel method, Gas grinding method, granulation-rolling method, extrusion molding-rolling method, spray-drying process etc.The maximum preparation method of current application is spray-drying process, its principle is that stock liquid spraying gun is dispersed into droplet, droplet forms ball shape under capillary effect, and by the mode that warm air (or other gas) directly contacts with droplet, and obtain a kind of drying process of powder granular products, can produce by continuous batch.
Lower primary school certain herbaceous plants with big flowers etc. are to Al
2o
3powder carries out the Al that spraying dry has prepared 20 ~ 100 μm
2o
3ceramic microsphere.Lu Youjun etc. are by obtaining the SiC ceramic microballoon that median size is 50 μm to SiC slurry spraying dry.Chinese patent " a kind of preparation method of diatomite-based porous ceramic microspheres " (application number: 201110228418.4, publication number: 102391011A, publication date: 2012-03-28), disclose a kind of preparation method of diatomite-based porous ceramic microspheres, take diatomite as main raw material, prepare porous ceramics microballoon by spraying dry.But the grain size of microballoon is difficult to control, and is difficult to practical requirement.
Existing electrostatic spray prepares the method for porous ceramics microballoon, what adopt is EFI liquid is carried out coaxial low temperature electrostatic spray obtain spherical matrix material, again spherical matrix material is sintered after lyophilize, obtained porous ceramics microballoon, this method is very high to the requirement of temperature, must carry out under the cold condition of-50 ~ 10 DEG C, and also very high to the requirement of equipment, part is a lot, and equipment is complicated.
Therefore, existing most of preparation method's complicated operation, microballoon preparation efficiency is low, is difficult to large-scale application.Although spray-drying process compares the preparation method with economic worth at present, its complex process, flow process is too much, and equipment is many, and the probability that is out of order is large, and floor space is large, and energy consumption is high, is also difficult to accurately control microspherulite diameter and porosity.
Summary of the invention
In view of this, in order to overcome above-mentioned problems of the prior art, the invention provides a kind of simple to operate, favorable repeatability, energy-efficient, accurately can control microspherulite diameter and porosity, the preparation method of micro-ceramic microballoon that can realize automatization, suitability for industrialized production, and the EFI solution used in preparation process and device.
In order to realize foregoing invention object, the present invention adopts following technical scheme:
For the preparation of an EFI solution for micro-ceramic microballoon, described EFI solution by mass ratio be the polyethersulfone of 1:3 ~ 6:3 ~ 6, N-Methyl pyrrolidone and yttria-stabilized zirconia form.
Wherein in some embodiments, described EFI solution by mass ratio be the polyethersulfone of 1:6:3, N-Methyl pyrrolidone and yttria-stabilized zirconia form.
Present invention also offers the method preparing micro-ceramic microballoon, take following technical scheme:
Prepare a method for micro-ceramic microballoon, comprise the following steps:
(1), EFI solution is prepared
Polyethersulfone to be mixed with N-Methyl pyrrolidone, 200-1000r/m mechanical stirring, and 60-90 DEG C of oil bath heated and stirred 0.5-6h, then adds yttria-stabilized zirconia powder, continue heated and stirred 6-24h, to be mixed evenly after obtain the EFI solution of EFI microballoon;
(2), electrostatic spray
The EFI solution prepared is joined in EFI syringe, voltage of supply is adjusted to 15 ~ 20kV, and driving pressure is adjusted to 0.1 ~ 0.6MPa, the mixed solution of filled with water, dehydrated alcohol or water and dehydrated alcohol in Receiving bin, carry out electrostatic spray, in receiving tank, obtain microballoon green compact;
(3), the sintering of microballoon green compact
With filtered on buchner funnel microballoon green compact, then at 80 ± 5 DEG C dry 1.5 ~ 3h, high temperature sintering, to obtain final product.
Wherein in some embodiments, described in step (2), voltage of supply is 20Kv, and described driving pressure is adjusted to 0.4MPa.
Wherein in some embodiments, the EFI syringe needle of EFI syringe described in step (2) is 15#, 18#, 21# or No. 25#, wherein 15# syringe needle internal diameter 1.37mm, 18# syringe needle internal diameter 0.84mm, 21# syringe needle 0.52mm, 25# syringe needle internal diameter is 0.26mm.
Wherein in some embodiments, filling with volume ratio in Receiving bin described in step (2) is the water of 1:1 and the mixed solution of dehydrated alcohol.
Wherein in some embodiments, described in step (3), the program of high temperature sintering is: be warmed up to 1000 DEG C from 50 DEG C, heating-up time 400min; 1400 DEG C are warmed up to, heating-up time 150min from 1000 DEG C; 120min is stopped at 1400 DEG C; 400 DEG C are cooled to, temperature fall time 120min from 1400 DEG C; Room temperature is cooled to from 400 DEG C.
Wherein in some embodiments, in step (3) at 80 DEG C dry 2-10h.
Present invention also offers the electric injection device for the preparation of micro-ceramic microballoon, take following technical scheme:
For the preparation of an electric injection device for micro-ceramic microballoon, described electric injection device comprises gas-powered system, electric field driven system and Receiving bin, and described gas-powered system is by the N be connected successively by conduit
2gas cylinder, pressure driver and EFI syringe form, described electric field driven system is made up of high-voltage power supply group, EFI syringe needle, foil electrode, the positive pole of described high-voltage power supply group is connected with EFI syringe needle by electrical lead, and the negative pole of described high-voltage power supply group is connected with foil electrode by electrical lead; Described EFI pinhead sleeve is located at the end of described EFI syringe, is provided with Receiving bin above described foil electrode, below EFI syringe needle.
Gas-powered system provides the EFI solution in pressure, push EFI syringe to spray from EFI syringe needle, and pressure range is at 0.1 ~ 0.6MPa; Electric field driven system forms electric field between EFI syringe needle and foil electrode, and charged EFI solution bursts under the effect of electrical forces, thus forms micron-sized drop.Strength of electric field is by the voltage-regulation of high-voltage power supply, and voltage range is at 15 ~ 20KV.
Wherein in some embodiments, the airway connecting described pressure driver and EFI syringe is connected with multichannel gas head, is often all connected with an EFI syringe on the way; The electrical lead connecting described EFI syringe needle and high-voltage power supply group is connected with plurality of voltages and coupling head.Described multichannel gas head can be four holes, seven apertures in the human head, 12 holes ... multichannel gas head, described plurality of voltages coupling head can be four holes, seven apertures in the human head, 12 holes ... plurality of voltages coupling head.
The EFI method that the present invention adopts, also known as electrostatic Spraying technique, utilizes the electrostatic force to polymers soln under high pressure static electricity, prepares polymer microsphere and complex microsphere.Its principle is: between EFI syringe needle and Receiving bin, set up a high tension electrostatic field, charged drop is under the effect of high tension electrostatic field, electrostatic field force can be formed at drop internal, when electrical forces reaches the surface tension enough overcoming drop while, will be there is unstable explosion in charged drop, form the drop of the micron level of dispersion.Drop falls into Receiving bin and forms spheroidal particle through inversion of phases.Compared with prior art, the present invention has following beneficial effect:
(1), the method for the micrometer level porous ceramic microsphere of preparation of the present invention adopts electrostatic spraying method, technique is simple, equipment is simplified, just automatic production can be realized at normal temperatures, the bead that EFI goes out is uniformly dispersed, soilless sticking, and EFI condition can be controlled, thus the size of fine adjustment microballoon and porosity;
(2), the method for the micrometer level porous ceramic microsphere of preparation of the present invention can adopt multiple EFI syringe and syringe needle EFI simultaneously, and thus working efficiency is higher; Whole technique only consumes electric energy, and thus preparation cost is low, and low in the pollution of the environment, is easy to apply.
Accompanying drawing explanation
Fig. 1 is the structural representation of the electric injection device for the preparation of micro-ceramic microballoon of embodiment 1;
Fig. 2 is the structural representation of the inhaler for the preparation of micro-ceramic microballoon of embodiment 7;
Reference numeral: 1, nitrogengas cylinder; 2, pressure driver; 3, EFI syringe; 4, EFI syringe needle; 5, Receiving bin; 6, foil electrode; 7, high-voltage power supply group; 8, multichannel gas head; 9, plurality of voltages coupling head; H, microballoon fall distance; V, EFI voltage.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, 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, be not intended to limit the present invention.
The reagent used in following examples is purchased from Shanghai Jing Chun biochemical technology limited-liability company.
Embodiment 1
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
First by PESF (polyethersulfone) and NMP (N-Methyl pyrrolidone) in mass ratio 1:6 add there-necked flask, 200r/m mechanical stirring, and 70 DEG C of oil bath heated and stirred 1h, add again with PESF (polyethersulfone) mass ratio be 3 YSZ (yttria-stabilized zirconia) powder, continue heated and stirred 12h, to be mixed evenly after obtain the EFI solution (PESF:NMP:YSZ=1:6:3) of EFI microballoon;
(2), electrostatic spray
Joined in 25# EFI syringe 3 by the EFI solution prepared, voltage of supply is adjusted to 20kV, and driving pressure is adjusted to 0.4MPa, and filled with water in Receiving bin 5 carries out electrostatic spray, obtains microballoon green compact in Receiving bin; Specifically comprise step:
a builds electric injection device
As shown in Figure 1, electric injection device is divided into two systems, and gas-powered system and electric field driven system, also comprise Receiving bin 5.
Gas-powered system is by N
2gas cylinder 1, pressure-driven setter 2 and EFI syringe 3 form, and are connected successively therebetween by airway; Electric field driven system is made up of EFI syringe needle 4, foil electrode 6 and high-voltage power supply group 7, the positive pole of high-voltage power supply group 7 is connected with EFI syringe needle 4 by electrical lead, the negative pole of high-voltage power supply group 7 is connected with foil electrode 6 by electrical lead, described EFI syringe needle 4 is sheathed on the end of described EFI syringe 3, above described foil electrode 6, is provided with Receiving bin 5 below EFI syringe needle 4.In this embodiment, EFI syringe needle is 25# syringe needle.
b EFI
Gas-powered system provides the EFI solution in pressure, push EFI syringe 3 to spray from EFI syringe needle 4, electric field driven system forms electric field between EFI syringe needle 4 and foil electrode 6, charged EFI solution bursts under the effect of electrical forces, and fall into the Receiving bin 5 of filled with water, charged EFI solution falls into Receiving bin 5 and immediately inversion of phases occurs, be frozen into microballoon form, thus form micron-sized microballoon green compact.EFI voltage V is by the voltage-regulation of high-voltage power supply group 7, and voltage range is at 20KV, and pressure range is at 0.4MPa.The microballoon of EFI syringe needle 4 and Receiving bin 5 falls distance h, namely EFI solution droplets fall distance, distance shorter, strength of electric field larger (E=U/d), while droplets fall be also subject to gravitational effect, the speed Vt=V of whereabouts
0+ gt, fall time is longer, and the speed Vt falling into drop during liquid level is larger.In this embodiment, drop fall distance range at 10cm.
Concrete EFI step is as follows:
B1, put up electric injection device as shown in Figure 1, EFI solution stirring well after pours EFI syringe 3 into, connect air duct fitting, screw, note preventing gas leakage;
B2, the positive pole of high-voltage power supply group 7 is clamped EFI syringe needle 4, negative pole clamps foil electrode 6;
The voltage-regulation button of b3, turn high-voltage power supply group 7, regulates required voltage.
B4, regulate the air pressure of pressure driver 2;
B5, press power initiation key, press the control valve of pressure driver 2, start EFI;
Necessary first closing presure driving mechanism 2 control valve when b6, EFI stop, the air pressure that pressure driver 2 produces is the Direct driver power that EFI solution sprays from EFI syringe needle 4, pressure controlled valve cuts out rear EFI and stops at once, although at this moment still have electric field between EFI syringe needle 4 electrode and foil electrode, do not have drop ejection.
B7, closedown high-voltage power supply group 7, pull up positive and negative electrode folder.
If b6, b7 sequence of steps is put upside down, first close high-voltage power supply group 7, closing presure driving mechanism 2 again, then to close in high-voltage power supply group 7 and in the time period that pressure driver 2 is not closed, EFI solution is had to spray from EFI syringe needle 4, and EFI solution can not be dispersed into the small droplets of micron level under the condition not having electric field action, thus can produce the huge microballoon of particle diameter and be mixed in receiving tank 5, contaminated samples.
(3), the sintering of microballoon green compact
After EFI terminates, by the microballoon green compact filtered on buchner funnel (the common qualitative filter paper of filter paper) in receiving tank 5, obtain ceramic microsphere green compact, oven drying 2h at putting into 80 DEG C again, after drying is complete, green compact are put into crucible, be placed in tube furnace high temperature sintering, sintering procedure terminates rear taking-up crucible, obtain the organism burnouted in microballoon green compact in porous ceramics microballoon sintering process, the microballoon after sintered presents vesicular structure).
Wherein, the specific procedure of high temperature sintering is as follows:
Program 1,50 DEG C → 1000 DEG C (400min), tube furnace is warmed up to 1000 DEG C from 50 DEG C, heating-up time 400min;
Program 2,1000 DEG C → 1400 DEG C (150min), tube furnace is warmed up to 1400 DEG C from 1000 DEG C, heating-up time 150min;
Program 3,1400 DEG C → 1400 DEG C (120min), tube furnace stops 120min at 1400 DEG C;
Program 4,1400 DEG C → 400 DEG C (120min), tube furnace cools to 400 DEG C from 1400 DEG C, temperature fall time 120min;
Program 5,400 DEG C → room temperature, lowers the temperature with stove.
Embodiment 2
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
With embodiment 1
(2), electrostatic spray
In this embodiment, EFI syringe needle has changed 21# syringe needle into, in other conditions, all identical with embodiment 1 (EFI solution is PESF:NMP:YSZ=1:6:3, microballoon falls distance for 10cm, high-voltage power supply group voltage is 20kV, driving pressure is adjusted to 0.4MPa, water receive bath) when start EFI.
(3), the sintering of microballoon green compact
With embodiment 1.
Embodiment 3
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
With embodiment 1
(2), electrostatic spray
In this embodiment, the distance (microballoon falls distance) of EFI syringe needle and Receiving bin liquid level is adjusted to 20cm, in other conditions, all identical with embodiment 1 (EFI solution is PESF:NMP:YSZ=1:6:3, EFI syringe needle is 25# syringe needle, high-voltage power supply group voltage is 20kV, driving pressure is adjusted to 0.4MPa, water receive bath) when start EFI.
(3), the sintering of microballoon green compact
With embodiment 1.
Embodiment 4
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
With embodiment 1
(2), electrostatic spray
In this embodiment, high-voltage power supply group voltage is 15kV, other conditions are all identical with embodiment 1, and (EFI solution is PESF:NMP:YSZ=1:6:3, EFI syringe needle is 25# syringe needle, microballoon falls distance for 10cm, driving pressure is adjusted to 0.4MPa, water receive bath) when start EFI.
(3), the sintering of microballoon green compact
With embodiment 1.
Embodiment 5
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
With embodiment 1
(2), electrostatic spray
In this embodiment, driving pressure is adjusted to 0.2MPa, other conditions are all identical with embodiment 1, and (EFI solution is PESF:NMP:YSZ=1:6:3, EFI syringe needle is 25# syringe needle, microballoon falls distance for 10cm, high-voltage power supply group voltage is 20kV, water receive bath) when start EFI.
(3), the sintering of microballoon green compact
With embodiment 1.
Embodiment 6
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
With embodiment 1
(2), electrostatic spray
In this embodiment, dehydrated alcohol is filled with by Receiving bin, water receives bath and changes ethanol reception bath into, other conditions are all identical with embodiment 1, and (EFI solution is PESF:NMP:YSZ=1:6:3, EFI syringe needle is 25# syringe needle, microballoon falls distance for 10cm, and driving pressure is adjusted to 0.4MPa, and high-voltage power supply group voltage is 20kV) when start EFI.
(3), the sintering of microballoon green compact
With embodiment 1.
Embodiment 7
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
With embodiment 1
(2), electrostatic spray
In this embodiment, dehydrated alcohol and quality will be filled with than the mixing solutions for 1:1 in Receiving bin, other conditions are all identical with embodiment 1, and (EFI solution is PESF:NMP:YSZ=1:6:3, EFI syringe needle is 25# syringe needle, microballoon falls distance for 10cm, driving pressure is adjusted to 0.4MPa, and high-voltage power supply group voltage is 20kV) when start EFI.
(3), the sintering of microballoon green compact
With embodiment 1.
Embodiment 8
A kind of method preparing micro-ceramic microballoon of the present embodiment, comprises the following steps:
(1), EFI solution is prepared
With embodiment 1
(2), electrostatic spray
In this embodiment, electric injection device is not identical with embodiment 1, as shown in Figure 2, airway between Bonding pressure driving mechanism 2 and EFI syringe 3 connects a multichannel gas head 8 (in this embodiment, be 4 holes), each road all connects an EFI syringe 3, realizes multi-channel parallel, also increase the pressure of pressure driver 2 simultaneously, make the pressure arriving each EFI syringe 3 control at 0.4MPa; Connection EFI syringe needle 4 with the electrical lead of high-voltage power supply group 7 are connected a plurality of voltages and coupling head 9 (in this embodiment, be 4 holes), each joint connects an EFI syringe needle 4, and realizing circuit is in parallel, and parallel connection does not need to strengthen electrode voltage again.The overall area strengthening foil electrode 6 and receiving tank 5, forms the electric injection device of EFI while of a multitube.
Other conditions are all identical with embodiment 1, and (EFI solution is PESF:NMP:YSZ=1:6:3, EFI syringe needle is 25# syringe needle, microballoon falls distance for 10cm, and driving pressure is adjusted to 0.4MPa, and high-voltage power supply group voltage is 20kV) when start EFI.
(3), the sintering of microballoon green compact
With embodiment 1.
Test example performance test
Measure the microspherulite diameter of the porous ceramics microballoon obtained of embodiment 1-8, porosity, measurement result is shown in Table 1.
Microspherulite diameter, the porosity of table 1 embodiment of the present invention 1-8 compare
As known from Table 1, after sintering, the particle diameter of ceramic microsphere depends primarily on EFI needle sizes, high-voltage power supply group voltage and driving pressure three parameters; Syringe needle internal diameter is larger, and the particle diameter of ceramic microsphere is larger, and voltage is higher, and the particle diameter of ceramic microsphere is less, and driving pressure is larger, and the particle diameter of ceramic microsphere is larger.Ceramic microsphere porosity depends primarily on sphere receiver bath solvent property and microballoon falls distance two parameters; The ceramic microsphere porosity receiving bath dehydrated alcohol is little, and fall distance larger, ceramic microsphere porosity is larger.As can be known from Table 1, the over-all properties of the porous ceramics microballoon of embodiment 1 is best.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1., for the preparation of an EFI solution for micro-ceramic microballoon, it is characterized in that, described EFI solution by mass ratio be the polyethersulfone of 1:3 ~ 6:3 ~ 6, N-Methyl pyrrolidone and yttria-stabilized zirconia form.
2. the EFI solution for the preparation of micro-ceramic microballoon according to claim 1, is characterized in that, described EFI solution by mass ratio be the polyethersulfone of 1:6:3, N-Methyl pyrrolidone and yttria-stabilized zirconia form.
3. prepare a method for micro-ceramic microballoon, it is characterized in that, use the EFI solution described in claim 1 or 2, comprise the following steps:
(1), EFI solution is prepared
Polyethersulfone to be mixed with N-Methyl pyrrolidone, 200-1000r/m mechanical stirring, and 60-90 DEG C of oil bath heated and stirred 0.5-6h, then adds yttria-stabilized zirconia powder, continue heated and stirred 6-24h, to be mixed evenly after obtain the EFI solution of EFI microballoon;
(2), electrostatic spray
The EFI solution prepared is joined in EFI syringe, regulating power source voltage is 15 ~ 20kV, and driving pressure is 0.1-0.6MPa, the mixed solution of filled with water, dehydrated alcohol or water and dehydrated alcohol in Receiving bin, carry out electrostatic spray, in receiving tank, obtain microballoon green compact;
(3), the sintering of microballoon green compact
With filtered on buchner funnel microballoon green compact, then at 80 ± 5 DEG C dry 1.5 ~ 3h, high temperature sintering, to obtain final product.
4. the method preparing micro-ceramic microballoon according to claim 3, is characterized in that, described in step (2), voltage of supply is 20kV, and described driving pressure is 0.4MPa.
5. the method preparing micro-ceramic microballoon according to claim 3, is characterized in that, the EFI syringe needle of EFI syringe described in step (2) is 15#, 18#, 21# or No. 25#.
6. the method preparing micro-ceramic microballoon according to claim 3, is characterized in that, filling with volume ratio in Receiving bin in step (2) is the water of 1:1 and the mixed solution of dehydrated alcohol.
7. the method preparing micro-ceramic microballoon according to any one of claim 3-6, is characterized in that, described in step (3), the program of high temperature sintering is: be warmed up to 1000 DEG C from 50 DEG C, heating-up time 400min; 1400 DEG C are warmed up to, heating-up time 150min from 1000 DEG C; 120min is stopped at 1400 DEG C; 400 DEG C are cooled to, temperature fall time 120min from 1400 DEG C; Room temperature is cooled to from 400 DEG C.
8. the method preparing micro-ceramic microballoon according to any one of claim 3-6, is characterized in that, in step (3) at 80 DEG C dry 2h.
9. for the preparation of micro-ceramic microballoon an electric injection device, it is characterized in that, described electric injection device comprises gas-powered system, electric field driven system and Receiving bin, and described gas-powered system is by the N be connected successively by conduit
2gas cylinder, pressure driver and EFI syringe form, described electric field driven system is made up of high-voltage power supply group, EFI syringe needle, foil electrode, the positive pole of described high-voltage power supply group is connected with EFI syringe needle by electrical lead, and the negative pole of described high-voltage power supply group is connected with foil electrode by electrical lead; Described EFI pinhead sleeve is located at the end of described EFI syringe, is provided with Receiving bin above described foil electrode, below EFI syringe needle.
10. according to claim 9 for the preparation of micro-ceramic microballoon electric injection device, it is characterized in that, the airway connecting described pressure driver and EFI syringe is connected with multichannel gas head, is often all connected with an EFI syringe on the way; The electrical lead connecting described EFI syringe needle and high-voltage power supply group is connected with plurality of voltages and coupling head.
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| CN109868058A (en) * | 2019-01-11 | 2019-06-11 | 上海交通大学 | Asymmetric hollow zirconic acid lanthanum microballoon enhancing silicon rubber insulating moulding coating and its application |
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| 杨乃涛: ""微管式固体氧化物燃料电池的制备及其性能研究"", 《中国博士学位论文全文数据库 工程科技II辑》 * |
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| CN105086454A (en) * | 2015-09-16 | 2015-11-25 | 苏州大学 | High-temperature resistance polyether sulfone nano-porous microspheres and preparation method thereof |
| CN109868058A (en) * | 2019-01-11 | 2019-06-11 | 上海交通大学 | Asymmetric hollow zirconic acid lanthanum microballoon enhancing silicon rubber insulating moulding coating and its application |
| CN110722813A (en) * | 2019-09-20 | 2020-01-24 | 上海松冒实业有限公司 | Device and method for preparing electrospray composite material |
| CN110722813B (en) * | 2019-09-20 | 2021-07-23 | 上海松冒实业有限公司 | Device and method for preparing electrospray composite material |
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| CN104529504B (en) | 2017-01-04 |
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