CN102464323A - Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma - Google Patents
Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma Download PDFInfo
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Abstract
The invention relates to a method for preparing a high-purity superfine zirconium boride powder by high-frequency plasma. A superhigh temperature heat source provided by a high-frequency plasma arc provides enough high temperature and energy for synthetic reaction; the electrodeless heating characteristic of the high-frequency plasma guarantees the high-purity quality of the product; particles freely deposit and grow in an airflow to obtain superfine particles with good dispersibility; and a reactor is designed to achieve a purpose of regulating product particle size. The zirconium boride powder prepared by the method provided by the invention has the advantages of high purity, good dispersibility and nano-scale size and is suitable for preparing high-temperature ceramic and compound material. The high-frequency plasma technology has a short flow and is suitable for large-scale production.
Description
Technical field
The invention relates to the method for preparing high pure and ultra-fine zirconium boride 99.5004323A8ure powder.In more detail, the present invention relates to a kind of method that adopts high frequency plasma prepared high pure and ultra-fine zirconium boride 99.5004323A8ure powder.
Background technology
Development along with modern technologies such as aviation, nuclear power, smelting new technologies; High-temperature structural material has been proposed more and more harsher requirement; Require material to have the good high-temperature performance to adapt to harsh operating environment, like anti-thermal shock, hot strength, solidity to corrosion, oxidation-resistance etc.Zirconium boride 99.5004323A8ure is as a kind of special high temperature ceramic material; Have characteristics such as HMP, HS, high firmness, favorable conductive thermal conductivity, excellent flame-retardant performance, thermotolerance, oxidation-resistance, erosion resistance and capture neutron; Obtained the concern of various countries' researchers gradually, obtained application more and more widely in high temperature fields such as aviation, metallurgy.The quality of zirconium boride 99.5004323A8ure powder is most important to the excellent zirconium boride ceramic product of processability.Therefore, low-cost, high-quality zirconium boride 99.5004323A8ure powder preparing is domestic and international important R&D direction.Because zirconium boride 99.5004323A8ure is difficult to sintering,, must adopt superfine zirconium boride 99.5004323A8ure powder in order to improve sintering quality.The zirconium boride 99.5004323A8ure powder of nanoscale, fine size, active high, easy sintering are important directions of zirconium boride 99.5004323A8ure powder development, have great exploitation value and application prospect.
Chinese patent CN 1152091C discloses the preparation method of a kind of zirconium diboride or TiB2 ultrafine powder; Use the self-spread synthesizing method principle; Adopt zircoium hydride (or titanium hydride) and pure boron to make raw material, behind ball mill mixing, pressed compact, vacuumize preheating, insulation, applying argon gas igniting reaction again; Reactant is carried out ball milling, obtain zirconium diboride or TiB2 ultrafine powder.
Chinese patent CN 100336723C discloses a kind of burning synthesis method of zirconium diboride micro mist; Basic material and thinner are prepared burden; Basic material is by weight percentage: ZIRCONIUM DIOXIDE 99.5: boric anhydride 31%～58%: magnesium powder 0%～25%: 25%～44%, and thinner is a zirconium diboride; Drying is 600～1200 minutes under the high-temperature vacuum condition, the mixture mechanical ball milling is mixed 1200～1500 minutes again; The blended powder is packed in the seal-off pressure container, and reactor drum adopts the recirculated water cooling, charges into protective atmosphere, and igniting makes it to take place self-propagating reaction; After the cooling Natural manganese dioxide is removed in product pickling in hydrochloric acid soln, remaining zirconium diboride obtains the finished product after washing, filtration, drying.
Chinese patent CN 100569644C discloses a kind of high purity ultra fine zirconium biboride powder and method thereof, and raw material contains zirconium oxychloride, boron carbide powder, activated carbon powder, and its mol ratio proportioning is: ZrOCl
2: B
4C: C=1: 0.4～0.8: 1.4～1.8.Press proportioning earlier with B
4C, C powder and H
2O mixes, and regulates the pH value, obtains B
4C and C powder mixing suspension; Zirconium oxychloride is dissolved in the deionized water, processes zirconyl chloride solution; Mixing suspension and zirconyl chloride solution is mixed, add ammoniacal liquor, make the abundant hydrolytic precipitation of zirconium oxychloride; With the suspensoid solid-liquid separation, NH is removed in washing
4+And Cl
-, sieve after the oven dry; Again powder is put into vacuum oven and react synthetic, 1500～1600 ℃ of synthesis temperatures are incubated 0.5～4 hour; Powder is levigate, sieves.
One Chinese patent application CN 01468918A discloses the preparation method of a kind of boride with high purity zirconium/hafnium boride powder and ceramic target thereof.This method is with high-purity Zr powder, and Hf powder and high-purity B powder are raw material, adopts from spreading method to prepare high-purity ZrB respectively
2And HfB
2Powder adopts the hot press forming technology of HTHP to prepare the zirconium boride 99.5004323A8ure/hafnium boride superhigh temperature ceramic target material of high-purity compact again, and the target specific density reaches 95～99%.
One Chinese patent application CN 101486577A discloses a kind of preparation method of nano zirconium diboride ceramic powder, following steps: 1) raw material is chosen: the mol ratio by Zr in the solubility zirconates and boron amorphous powder is 1: 3～1: 5, chooses; 2) adopt one of following two kinds of methods: a) coprecipitation method becomes glue, obtains xerogel; B) sol-gel method becomes glue, forms xerogel; 3) precursor powder preparation; 4) synthetic fast: inserting in the big current response synthesizer, is vacuum or protection of inert gas in the graphiote reactor; Graphiote reactor is directly applied big electric current, be heated rapidly to 800～1500 ℃ with the heat-up rate of 50～500 ℃/min, soaking time is 0～60 minute, powdered sample; 5) chemical treatment; Obtain nano zirconium diboride ceramic powder.
USP 4414188 discloses a kind of ZrB
2The preparation method of powder is through ZrCl
4Or ZrCl
2, boron halogenide and Al or Mg under molten salt bath, react and obtain ZrB
2Salt bath comprises KCl and NaCl, and temperature is 540 ℃ to 660 ℃.
In general, the main preparation methods of zirconium boride ceramic powder has direct synthesis technique, carbon or norbide reduction method, electrolysis to contain melting salt method, self propagating high temperature synthesis method, mechanochemical reaction of zirconium white and boron oxide etc.In above-mentioned several kinds of preparing methods, direct synthesis technique powder purity is high, but expensive raw materials, granularity is thick, and is active low, is unfavorable for the processing of sintering and post-treatment; Carbon in the suitability for industrialized production or norbide reduction method raw materials cost are low, and main drawback is that energy consumption is high, the production cycle is long, and the technology cost is high; Electrolytic process also relatively is fit to suitability for industrialized production, but introduces impurity easily, and product purity is not high, also will prevent zirconium boride 99.5004323A8ure sintering in process of production; Self propagating high temperature synthesis method process is simple, and speed of response is fast, and the time is very short; Energy consumption is minimum, and synthetic powder is active high, helps sintering and post-treatment and handles; But it is too fast, wayward that weak point is its speed of response, and reaction is carried out not really complete sometimes; Corresponding impurity also can be many, and its reaction process, product structure and performance all are not easy accurate control.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing high pure and ultra-fine zirconium boride 99.5004323A8ure powder; Prepared zirconium boride 99.5004323A8ure powder has characteristics such as purity height, fine size, narrow diameter distribution, and said method has characteristics such as adaptability to raw material is strong, industrial scale flexible, suitable suitability for industrialized production.
For realizing the foregoing invention purpose, proposed to adopt high frequency induction thermal plasma to prepare the novel method of high pure and ultra-fine zirconium boride 99.5004323A8ure powder.The ultrahigh-temperature thermal source that the high frequency induction thermal plasma arc provides is that building-up reactions provides enough temperature and energy; Electrodeless heat characteristic has guaranteed high-purity quality of product; Particle unhindered settling growth in air-flow can obtain disperseing nano particle preferably, can reach the purpose of control product particle size through reactor design.High frequency induction thermal plasma has that energy density is big, temperature is high and characteristics such as the cooling gradient is big, and it belongs to electrodeless heating; Can avoid electrode fouling; And plasma reaction system atmosphere is controlled, therefore can be used for preparing the higher nano-powder of purity requirement.
The main process of present method is in plasma reaction device, to carry out.Plasma reaction device is as shown in Figure 1, mainly comprises plasma generator (high frequency plasma power supply 1 and plasmatorch 2), plasma reactor 3, charging system 4, cooling system 5, gathering system 6.When high frequency plasma power supply 1 applies high-frequency electric field on ruhmkorff coil 11; (like electrical spark etc.) central gas (plasma body working gas) partial ionization for a certain reason; The charged particle that produces is done high-speed motion under the effect of high frequency alternating electromagnetic field; The collision gas atom makes it rapid, a large amount of ionization, forms the avalanche type discharge; Ionized gas forms the eddy current of closed annular on perpendicular to the cross section of field direction; In ruhmkorff coil, form the secondary coil be equivalent to X-former and with the ruhmkorff coil coupling that is equivalent to primary winding, the high temperature that this high frequency induction current produces is again with gas heating, ionization, and forms the stabilized plasma arc of a torch-like at the mouth of pipe.Central gas is often selected argon gas for use, also can select other gas according to reaction system, and neutral atmosphere can be selected gases such as nitrogen for use, and reducing atmosphere can be selected gases such as hydrogen, ammonia for use, and oxidizing atmosphere can be selected gases such as oxygen, air for use.Limit gas is mainly used in cooling protection plasma reactor 3, and limit gas can be selected the gas the same with central gas for use, also can select the cheap gas that does not influence reaction for use, and the throughput ratio of central gas and limit gas is generally 1: 3～6.After forming stable plasma arc; Raw material is sent in the plasma reactor 3 through charging system 4 by carrier gas; Under the plasma heat, be transported in the cooling system 5 after the reaction; Reacted product is collected through gathering system 6, removes the soluble impurity in the product through conventional washing drying process in case of necessity.Can control the residence time of raw material in plasma reactor through control carrier gas gas speed, this residence time was generally 0.08～1 second.Be to strengthen the mass transport effect, can be in device increase pumped vacuum systems (not shown) make and keep the certain vacuum degree in the device.When the gas usage quantity is big, can increase the gas-circulating system (not shown), with the tail gas recycle to reduce cost.In tail gas, contain directly emission gases (like chlorine, hydrogenchloride), should increase tail gas absorption system (not shown) with qualified discharge.Through structure of reactor design or adjusting processing parameter, change the reaction product process of cooling and can control the product cut size size.The structure of reactor design example can reduce product cut size as feed cold gas at plasma arc wake flame place, increases lagging facility at the reactor drum outer wall and can increase product cut size.The plasma reaction device industrial scale is flexible, and high frequency electric source power is determined by industrial scale, can between thousands of watts to hundreds of kilowatts, regulate.
High frequency plasma of the present invention prepares the method for high pure and ultra-fine zirconium boride 99.5004323A8ure powder to carry out according to the following steps:
(1) central gas is formed plasma arc by high frequency electric source ionization, feeds limit gas;
(2) under carrier gas was carried, boracic and zirconic raw material got into plasma reactor continuously;
(3) raw material that gets into plasma reactor reacts in the high-temperature zone;
(4) reaction product gets into cooling system deposition growing formation superfine powder after leaving high temperature reaction zone;
(5) powder gets into product collection system under gas drives;
(6) product of collecting obtains the zirconium boride 99.5004323A8ure powder through the washing drying.
In the above-mentioned steps (1), central gas can be argon gas or hydrogen, and limit gas can be the mixed gas of nitrogen, hydrogen or rare gas element and hydrogen.
In the above-mentioned steps (2), carrier gas can be the mixed gas of hydrogen or rare gas element and hydrogen.
In the above-mentioned steps (2), the boracic raw material can be boron-containing compounds such as boron trioxide, boric acid, boron trichloride, also can be boron simple substance; Zirconium-containing material can be zirconium-containing compounds such as ZIRCONIUM DIOXIDE 99.5, zirconium tetrachloride, zirconium oxychloride, also can be metal zirconium.The reinforced ratio of boracic raw material and zirconium-containing material is generally according to stoichiometric ratio (being the coefficient ratio in the chemical equation), and the ratio (be no more than stoichiometric ratio 2 times) that also can on the stoichiometric ratio basis, suitably increase a kind of raw material is to improve the yield of another kind of raw material.
In the above-mentioned steps (3), the high-temperature zone comprises plasma generation district and wake flame district, comprises that also other heating approach that adopt beyond the above-mentioned plasma body provide high-temperature area and soak zones.
In the above-mentioned steps (4), product deposition growing process can and be regulated the cooling conditions control in the processing parameter through reactor design.
In the above-mentioned steps (5), gathering system comprises the mode of cyclonic separation and gas solid separation such as cloth bag separates.
In the above-mentioned steps (6), products therefrom is removed soluble impurity and can be realized with absolute ethanol washing is dry more at last through using the deionized water repetitive scrubbing.
The resulting zirconium boride 99.5004323A8ure powder of the present invention purity is high, can reach more than the 99wt%; Fine size can be regulated in 10～500nm scope; Particles dispersed property is good, narrow diameter distribution.Preparation technology of the present invention is simple, good reproducibility, and adaptability to raw material is strong, and industrial scale is flexible, and the zirconium boride 99.5004323A8ure powder of preparation is applicable to preparation pyroceramic and high temperature composite.
Description of drawings:
Fig. 1 is the plasma reaction device synoptic diagram.
Fig. 2 is the XRD spectra of embodiment 1 product powder.
Fig. 3 is the stereoscan photograph of embodiment 1 product powder.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified.
High frequency plasma prepares nanometer zirconium boride 99.5004323A8ure powder and comprises 6 steps.The first step: the atmosphere displacement at first feeds central gas (argon gas or hydrogen) with the air in the displacement apparatus, for building-up reactions provides oxygen-free environment in plasma device; Second step: the starting the arc, supply with the certain hunting power of ruhmkorff coil through electrical power control cabinet, and use electrical spark striking, plasma arcs to form feeding limit, back gas from plasma torch is outside, can make through vacuum system and keep the certain vacuum degree in the device.The 3rd step: reinforced, behind plasma arcs steady running number minute, reaction system inside has reached thermal equilibrium basically, begins to feed in raw material through charging system, and feed rate can be through carrier gas (mixed gas of hydrogen or rare gas element and hydrogen) rate-controlling.The 4th step: blow-out, stop to rerun several minutes after reinforced, blow-out then should continue to feed central gas and do protection gas after the blow-out, until system cools, with the superfine powder that prevents to generate under hot conditions by airborne oxygen oxidation.The 5th step: collect product, open collector and reactor drum after the system that treats is cooled off fully and carry out the product collection.The 6th step: the washing drying prods, with the soluble impurity in the deionized water repetitive scrubbing product, use absolute ethanol washing at last, dry in baking oven.
Product to after handling carries out thing phase, oxygen level, sreen analysis, and the result shows, adopts the zirconium boride 99.5004323A8ure powder purity of high frequency plasma prepared higher, and oxygen level is less than 1%, even particle size distribution, and particle size can be regulated and control in the 10-500nm scope.Adopt the XRD spectra of the zirconium boride 99.5004323A8ure powder of high frequency plasma prepared to see accompanying drawing 2, adopt the stereoscan photograph of the zirconium boride 99.5004323A8ure powder of high frequency plasma prepared to see accompanying drawing 3.
Embodiment 1
Adopting boron trichloride and zirconium tetrachloride is raw material, prepares ultra-fine zirconium boride 99.5004323A8ure powder through high frequency plasma hydrogenation synthetic approach.Chemical reaction is shown below.
2BCl
3+ZrCl
4+5H
2→ZrB
2+10HCl
With hydrogen is carrier gas, and gaseous state boron trichloride and gaseous state zirconium tetrachloride are added in the plasma reactor, and wherein the ratio of boron trichloride and zirconium tetrachloride is 2: 1 ratio adding according to the ratio of amount of substance.Experimentation keeps that vacuum tightness is 200Pa in the system.Tail gas is discharged after sodium hydroxide solution absorbs.Synthetic product obtains ultra-fine zirconium boride 99.5004323A8ure through washing drying, and particle size is 30-60nm.
Embodiment 2
Adopting boric acid and zirconium white is raw material, prepares ultra-fine zirconium boride 99.5004323A8ure powder through high frequency plasma hydrogenation synthetic approach.Chemical reaction is shown below.
2H
3BO
3+ZrO
2+5H
2→ZrB
2+8H
2O
With hydrogen is carrier gas, and boric acid and zirconium white are added in the plasma reactor, and its mesoboric acid and zirconic ratio are that 2: 1 ratio adds according to the ratio of amount of substance.Experimentation is introduced cooling gas at plasma arcs wake flame place, keeps that vacuum tightness is 1kPa in the system.Synthetic product obtains ultra-fine zirconium boride 99.5004323A8ure through washing drying, and particle size is 10-40nm.
Embodiment 3
Adopting boron trioxide and ZIRCONIUM DIOXIDE 99.5 is raw material, prepares ultra-fine zirconium boride 99.5004323A8ure powder through high frequency plasma hydrogenation synthetic approach.Chemical reaction is shown below.
B
2O
3+ZrO
2+5H
2→ZrB
2+5H
2O
Being 1: 1 ratio ball mill mixing with boron trioxide and ZIRCONIUM DIOXIDE 99.5 in the ratio of amount of substance at first, is carrier gas with the mixed gas of hydrogen and argon gas, and solid material is added the plasma arcs zone.Reactor wall adds attemperator.Synthetic product obtains ultra-fine zirconium boride 99.5004323A8ure through washing drying, and particle size is 50-100nm.
Embodiment 4
Adopting boron powder and ZIRCONIUM DIOXIDE 99.5 is raw material, prepares ultra-fine zirconium boride 99.5004323A8ure powder through high frequency plasma hydrogenation synthetic approach.Chemical reaction is shown below.
2B+ZrO
2+2H
2→ZrB
2+2H
2O
Being 2: 1 ratio ball mill mixing with boron powder and ZIRCONIUM DIOXIDE 99.5 in the ratio of amount of substance at first, is carrier gas with hydrogen, and solid material is added the plasma arcs zone.Reactor wall adds insulation and heating unit, and experimentation keeps that vacuum tightness is 500Pa in the system.Synthetic product obtains ultra-fine zirconium boride 99.5004323A8ure through washing drying, and particle size is 100-500nm.
Embodiment 5
Adopting boric acid and zirconium oxychloride is raw material, prepares ultra-fine zirconium boride 99.5004323A8ure powder through high frequency plasma hydrogenation synthetic approach.Chemical reaction is shown below.
2H
3BO
3+ZrOCl
2·8H
2O+5H
2→ZrB
2+15H
2O+2HCl
Being 2: 1 ratio ball mill mixing with boric acid and zirconium oxychloride in the ratio of amount of substance at first, is carrier gas with the mixed gas of hydrogen and argon gas, and solid material is added the plasma arcs zone.Reactor wall adds insulation and heating unit, and experimentation keeps that vacuum tightness is 2kPa in the system.Tail gas is discharged after sodium hydroxide solution absorbs.Synthetic product obtains ultra-fine zirconium boride 99.5004323A8ure through washing drying, and particle size is 100-500nm.
Claims (10)
1. a high frequency plasma prepares the method for high pure and ultra-fine zirconium boride 99.5004323A8ure powder; It is characterized in that; The preparation process is carried out in plasma reaction device; Said plasma reaction device comprises high frequency plasma power supply (1), ruhmkorff coil (11), plasmatorch (2), plasma reactor (3), charging system (4), cooling system (5) and gathering system (6), and said preparation process comprises the following steps:
A) in plasma reaction device, feed central gas; Open high frequency plasma power supply (1) after draining the air in the device; Adopt electrical spark striking outside plasmatorch (2), feed limit gas, boracic and zirconic raw material are through charging system (4) is transported to plasma reactor (3) by carrier gas in;
B) raw material that gets into plasma reactor (3) reacts in the high-temperature zone;
C) reaction product gets into cooling system (5) deposition growing formation superfine powder after leaving high temperature reaction zone;
D) powder gets into gathering system (6) under gas drives;
E) product of collecting obtains the zirconium boride 99.5004323A8ure powder through the washing drying.
2. method according to claim 1 is characterized in that, said carrier gas is the mixed gas of hydrogen or rare gas element and hydrogen.
3. method according to claim 1 is characterized in that, said central gas is argon gas or hydrogen.
4. method according to claim 1 is characterized in that, the throughput ratio of said central gas and limit gas is 1: 3～6.
5. method according to claim 1 is characterized in that the boracic raw material can be boron-containing compounds such as boron trioxide, boric acid, boron trichloride, also can be boron simple substance; Zirconium-containing material can be zirconium-containing compounds such as ZIRCONIUM DIOXIDE 99.5, zirconium tetrachloride, zirconium oxychloride, also can be metal zirconium.
6. method according to claim 1 is characterized in that, the raw material that gets into plasma reactor (3) can be solid, gas or liquid; Raw material can add after the pre-mixing, also can add respectively.
7. method according to claim 1 is characterized in that, said raw material is 0.08～1 second in the residence time of plasma reactor (3).
8. method according to claim 1 is characterized in that said plasma reaction device also comprises pumped vacuum systems.
9. method according to claim 1 is characterized in that, introduces cooling gas at the plasma tail flame place.
10. method according to claim 1 is characterized in that, outside plasma reactor (3) wall, increases insulation and/or heating unit.
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