CN106045526A - Method for preparing ceramic powder through liquid-state CO2 - Google Patents

Abstract

The invention provides a method for preparing ceramic powder through liquid-state CO2. The method comprises: a) introducing liquid-state CO2 into a blasting cylinder to make a ceramic body be immersed in the liquid-state CO2 to achieve a saturated state; b) placing the blasting cylinder into a soil pit, filling soil, and compacting; and c) detonating the blasting cylinder. According to the present invention, the particle size distribution data of the ceramic powder obtained by using the method is close to the particle size distribution data of the high-performance ceramic; and the alkaline solution adding in the grinding process of the conventional method is eliminated, the process is simple, the blasting cylinder can be reused, and the price of the liquid-state CO2 is cheap, such that the further optimization and promotion can be performed on the basis of the method so as to expand the proportion of the fine particle size particles.

Description

A kind of liquid CO2The method preparing ceramic powder

Technical field

Present invention relates particularly to a kind of application liquid CO₂The method preparing ceramic powder.

Background technology

The method having multiple manufacture ceramic powder at present, is broadly divided into comminuting method and synthetic method.Comminuting method mainly uses Various mechanical crushing methods, this method is difficult to obtain 1 μm particles below, and is easily introduced impurity.Synthetic method is at atom, molecular water By reaction, nucleation on Ping, grow up, collect and process and obtain.The grain refine of ceramic powder contributes to obtaining high-performance Aplitic texture and greatly reduce sintering temperature, thus produce huge economic benefit, table 1 lists several frequently seen mineral Grain size and the relation of increment multiple.Studying at present and applying more new ceramic material is Si₃N₄、SiC、ZrO₂、Al₂O₃With BaTiO₃、Si₃N₄And SiC.Wherein Al₂O₃It it is one of material of usage amount maximum in current new ceramics.In superfine powder preparation Exist common problem be: crush efficiency is low, energy consumption is high, production cycle length, can not serialization, powder particle size do not reach use want Asking and concordance is poor, powder is contaminated seriously.The imagination of powder body development: pay attention to utilizing raw ore directly to prepare powder body is straight with raw ore Connect and prepare the effective ways that high pure and ultra-fine powder body is reduction cost, used clay, Alumina directly to prepare superfine high-purity The Al of degree₂O₃Powder body.

Rise in value after table 1 mineral superfine powder is broken multiple (1998)

When preparing high performance ceramic material, typically require that the granularity of raw material is less than l μm.If the fineness of raw material reaches to receive Meter level, then the pottery made is referred to as nano ceramics, and performance is more excellent, is the tidemark of current ceramic material development.One As advanced ceramic glaze require without or as far as possible few containing the granule more than 15 μm, and the glaze after superfine grinding is equal because of fine size Even, make the glaze smooth planar of ceramic product, glossiness is high, and pin hole is few, and color and luster is more bright-coloured, and the glaze used on product is also Few.Therefore, the Al of high-purity, nanoscale is obtained by continuous operations mode₂O₃Powder material will be our target.

High pressure pneumatic component method is the initial stage sixties to begin one's study application in the country that some mining industries such as the U.S. are flourishing A kind of physics blasting method, Ai Duo Ces Co., Ltd of the U.S. has succeeded in developing liquid CO at first₂Explosive cartridge.High pressure pneumatic component The pressure of pressure ratio explosive blasting is little, about the 1/3 of black powder, the 1/6 of nitrolite, high pressure pneumatic component pressure rise relative to Explosive is more slowly and the high pressure persistent period is longer, more applicable to broken porous fragility medium, has the most direct fragmentation effect.

Domestic scholars has carried out substantial amounts of experiment work, and Guo Zhixing (1994) utilizes liquefaction CO₂As transmission brisance Medium, before explosion will liquefaction CO₂It is filled with explosive cartridge, passes through electrode and heating element heater during work by CO₂Heating makes its pressure increase Add to a certain extent, thus break through explosive cartridge end shear dish, the CO of the rapid expanding that makes to be heated₂Valve by explosive cartridge end Discharge, provide aerodynamic force and thrust for explosion matter, explosion matter cubical expansion is opened.Du Yukun etc. (2012) have carried out supercritical CO₂Jet breaks rock experimental study, and supercritical carbon dioxide fluid has close to liquid high-density with close to the spy of gas low-viscosity Property, surface tension is little, thus has preferably flowing, infiltration and mass-transfer performance.Confirm supercritical CO₂Can effectively reduce brokenly rock door Limits pressure, large volume crushes to cause rock to occur.

As it is shown in figure 1, when temperature is higher than 31.04 DEG C, and pressure is higher than 7.38MPa, is in liquid CO of Fig. 1 above-critical state₂ Just good dissolving, permeability it are provided with；Density is close with liquid, big two orders of magnitude than general gas flow；Viscosity is approximately equal to The numerical value of gas, diffusion coefficient hundreds times bigger than liquid.

Chinese patent CN 204461254 U discloses a kind of carbon dioxide demolition set.It is specially a kind of carbon dioxide quick-fried Broken cylinder.

Above-mentioned liquid CO₂Broken rock device, very well embodies liquid CO₂The moment volume that phase transition process produces expands into The characteristic of the broken rock of row, and achieve preferable effect.

Summary of the invention

It is an object of the invention to provide a kind of operation utilization simple, repeatable, low price and ceramic powder particle diameter to exist The micron-sized method preparing ceramic powder.

In order to solve the problems referred to above, the present invention provides a kind of liquid CO₂The method preparing ceramic powder, including walking as follows Rapid:

A) in described explosive cartridge, it is filled with liquid CO₂, make described ceramic body immerse liquid CO₂Reach saturated；

B) described explosive cartridge is put in heatable adobe sleeping platform, and fill compaction；

C) described explosive cartridge is ignited.

Further, described ceramic body is aluminium oxide.

Further, described step a) particularly as follows:

It is filled with liquid CO in described explosive cartridge₂, pressure is set as 10Mpa, and temperature is-10 °, makes described ceramic body immerse Liquid CO₂Reach saturated.

Further, described step b) particularly as follows:

Described explosive cartridge is connected initiation control device by lead-in wire, is then put in heatable adobe sleeping platform, and fill compaction.

Relative to prior art, the present invention has a following technique effect:

Adopt the particle size distribution data closely high-performance ceramic of the ceramic powder being obtained by the present invention, the method Saving the process of lapping adding aqueous slkali in existing conventional method, operation is simple and the repeatable utilization of explosive cartridge, and liquid CO₂Valency Lattice are cheap.Therefore can optimize further on the basis of the method and promote, expand fine grain granule accounting.

Accompanying drawing explanation

Fig. 1 is carbon dioxide three-phase diagram；

Fig. 2 is the photo of block aluminium oxide before explosion；

Fig. 3 is the photo of the alumina powder after explosion；

Fig. 4 is alumina powder grading curve；

Fig. 5 is bauxite component curve.

Detailed description of the invention

Below in conjunction with accompanying drawing, embodiments of the invention are described in detail.It should be noted that do not conflicting In the case of, the embodiment in the application and the feature in embodiment can mutual combination in any.

Embodiment one:

In view of liquid CO₂Volume-expanding characteristics higher when having preferable permeability and a phase transformation, the present invention utilizes China specially Cardox blaster disclosed in profit CN 204461254 U, it is provided that a kind of liquid CO₂The method preparing ceramic powder, including such as Lower step:

A) in explosive cartridge, liquid CO it is filled with₂, pressure is set as 10Mpa, and temperature is-10 °, makes ceramic body immerse liquid CO₂ Reach saturated；

B) explosive cartridge is connected initiation control device by lead-in wire, be then put in heatable adobe sleeping platform, and fill compaction；

C) explosive cartridge is ignited.

After explosion terminates, block aluminium oxide is by efflorescence, as shown in Figure 3.

Due to liquid CO₂Easily penetrating into block aluminium oxide intracell, then heated up by heater, high voltage transient breaks up Burst disk, liquid CO₂Gaseous state CO it is converted in 5-7ms₂, volume meeting instantaneous expansion 500-600 times, include liquid CO₂Bulk Aluminium oxide is broken for powder under bigger barometric gradient effect.Similar with above-mentioned scholar's process of the test, the difference of the present invention It is to be placed in inside high-pressure bottle by explosion matter, utilizes liquid CO₂Easily permeate and gasify volumetric expansion dual function, explosion-proof The moment that sheet breaks, under higher barometric gradient effect, penetrate into block liquid CO within aluminium oxide₂Drastically expand, cause The efflorescence of block aluminium oxide.

By above-mentioned ongoing liquid CO₂Carry out ceramic powder preparation and laser particle size analysis is tested, by alumina powder End is put in water and is disperseed, and then draws 5ml solution with dropper, instills in laser particle analyzer dispersion liquid, experimental test granule Size distribution curve is as shown in Figure 4.Can be seen that, particle diameter integrated distribution is interval in 20-40 μm.As it is shown in figure 5, particle diameter is less than 83.5 μm account for 90%, this particle size distribution data distance high-performance ceramic or nano ceramics also have a certain distance, but the method saves Removing to add in existing conventional method the process of lapping of aqueous slkali, operation is simple and the repeatable utilization of explosive cartridge, adds liquid CO₂Valency Lattice are cheap.Therefore can optimize further on the basis of the method and promote, expand fine grain granule accounting.

The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies Change, equivalent, improvement etc., should be included within the scope of the present invention.

Claims (4)

1. liquid CO₂The method preparing ceramic powder, it is characterised in that comprise the steps:

A) in described explosive cartridge, it is filled with liquid CO₂, make described ceramic body immerse liquid CO₂Reach saturated；

B) described explosive cartridge is put in heatable adobe sleeping platform, and fill compaction；

C) described explosive cartridge is ignited.

2. the method for claim 1, it is characterised in that:

Described ceramic body is aluminium oxide.

3. method as claimed in claim 2, it is characterised in that described step a) particularly as follows:

It is filled with liquid CO in described explosive cartridge₂, pressure is set as 10Mpa, and temperature is-10 °, makes described ceramic body immerse liquid CO₂Reach saturated.

4. method as claimed in claim 3, it is characterised in that described step b) particularly as follows:

Described explosive cartridge is connected initiation control device by lead-in wire, is then put in heatable adobe sleeping platform, and fill compaction.