CN106694905A - Preparation method and preparation devices for nanometer beryllium powder - Google Patents
Preparation method and preparation devices for nanometer beryllium powder Download PDFInfo
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- CN106694905A CN106694905A CN201710123461.1A CN201710123461A CN106694905A CN 106694905 A CN106694905 A CN 106694905A CN 201710123461 A CN201710123461 A CN 201710123461A CN 106694905 A CN106694905 A CN 106694905A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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Abstract
The invention discloses a preparation method and preparation devices for nanometer beryllium powder and belongs to the technical filed of beryllium powder preparing. The preparation method comprises the steps that carrying gas is adopted to convey organic beryllium etherate steam from a source bottle to a heated constant-temperature mineral oil through a pipeline; organic beryllium etherate gaseous molecules are pyrolyzed in the mineral oil to generate BeH2, and by-products of isobutene and diethyl ether are used as tail gas to be discharged; in the mineral oil, the BeH2 is pyrolyzed again and dehydrogenized to generate beryllium; and the mineral oil is separated and dried to obtain the nanometer beryllium powder. The preparation devices comprise the source bottle, a reacting bottle, a bubbling bottle and a condensing device. The source bottle is connected with the reacting bottle and further communicates with a gas inlet pipe. The reacting bottle further communicates with the condensing device. The other end of the condensing device communicates with the bubbling bottle through a second pipeline. According to the prepared beryllium powder, the diameter is smaller, specifically, the diameter is less than 65 nm; the carbon impurity content is low, specifically, the carbon impurity content is less than 0.2 at%; and the total amount of the metal impurities in the finally obtained beryllium powder is less than 12 ppm.
Description
Technical field
Organic beryllium etherate is carried using carrier gas the present invention relates to a kind of nanometer of preparation method of beryllium powder, more particularly to one kind
The method that steam prepares nanometer beryllium powder to pyrolysis in the mineral oil of heated constant temperature.
Background technology
Beryllium is a kind of rare light metals, with many special performances, is widely used in many important engineering fields, for example
Inertial navigation, optical system, guided missile, satellite, spacecraft and aviation etc..Current metallic beryllium is substantially and is obtained by powder metallurgy
, because beryllium ingot casting contains substantial amounts of hole, microscopic structure is thick grainiess, even if after working process, crystal grain
, also greater than 100 μm, as a result the mechanical performance of beryllium ingot casting is excessively poor for degree.Therefore the manufacture of beryllium part can only use powder metallurgic method, i.e.,
Beryllium ingot casting is lathed bits, powder is then made, subsequent working process is used further to.
With the development of science and technology, high intensity particularly of new generation, the appearance of high ductibility beryllium material, the preparation to beryllium powder
Propose tightened up requirement.The granularity of beryllium powder, chemical composition, physical property, processing performance are to its consolidation process and final
Properties of product have great influence.The preparation of beryllium powder is usually to use mechanical means, mainly has disc grinder, ball milling, impact to grind
Mill, gas atomization etc..The prevailing technology of current beryllium powder production is impact grinding method, and the beryllium Powder Particle Size that it is obtained is in some tens of pm
Magnitude.The method is difficult to be greatly reduced again the particle diameter of beryllium powder, and complex process equipment, high cost, grinds repeatedly, the time
Long, often, go out that powder temperature is high, degree of oxidation is high.Grinding equipment contact introduces impurity.
Be assigned to organic beryllium etherate in the mineral oil of heated constant temperature using microlayer model generator by present applicant
Pyrolysis has obtained nanometer beryllium powder, and its specific method such as number of patent application is announced by 201610307415.2 Chinese patent application
, the particle diameter of beryllium powder can be reduced to nanoscale by this method, and most thin diameter can reach 500nm.This method is used
The mode of microlayer model sample introduction, relatively natural drop, although microlayer model very little, is still by a large amount of organic beryllium molecule cohesions
Into the particle diameter of the beryllium powder for obtaining is difficult to further reduction.Meanwhile, there is thermograde in microlayer model, pyrolysis temperature is uneven,
The pyrolysis temperature of organic beryllium molecule of drop internal is low compared with organic beryllium molecule of droplet surface, causes the organic beryllium in part not exclusively hot
Solution generation carbon compound, carbon impurity is difficult to remove in beryllium powder, and in the beryllium powder of gained, carbon impurity content is 1.5at% (atomicities
Percentage composition), carbon impurity content higher have impact on the quality and performance of beryllium powder, and metal impurities total amount is 20ppm or so.
The content of the invention
An object of the present invention, in that a kind of nanometer of preparation method of beryllium powder is provided, to solve the above problems.
To achieve these goals, the technical solution adopted by the present invention is such：A kind of nanometer of preparation method of beryllium powder,
Comprise the following steps：
A () heats and constant temperature mineral oil；
B () organic beryllium etherate steam is pipelined to the heated constant temperature of step (a) using carrier gas from source bottle
Mineral oil in；
C () organic beryllium etherate gaseous molecular is pyrolyzed generation BeH in mineral oil2, accessory substance isobutene, ether are used as tail
Gas is discharged；
(d) in mineral oil, BeH2The dehydrogenation of reheating solution generates beryllium；
E () separates mineral oil, and be dried to obtain a nanometer beryllium powder.
Organic beryllium etherate that the present invention realizes molecular state is pyrolyzed in mineral oil.
As preferred technical scheme：The mineral oil is n-dodecane or n-tridecane or n-tetradecane.
As preferred technical scheme：Step (a) heated constant temperature is to 200 DEG C -250 DEG C.
As preferred technical scheme：Organic beryllium etherate is glucinum ethyl etherate, Di-tert-butyl beryllium second
Ether complex.
As preferred technical scheme：Step (b) carrier gas is ultrapure argon or superpure nitrogen.
It is further preferred that purity >=99.9999% of the ultrapure argon or superpure nitrogen.
As preferred technical scheme：Step (b) carrier gas flux is 0.01slm-5slm.In the present invention, unless special
Do not mentionlet alone bright, " slm " refers to the flow of 1L/min under standard state.
As preferred technical scheme：Step (b) the source bottle and pipeline are heated, and the temperature that pipeline is heated
Temperature with source bottle heating is consistent, and the heating-up temperature of preferably described source bottle and pipeline is 20 DEG C -50 DEG C.
As preferred technical scheme：The preparation process of methods described is in the middle and high pure inert gas environment of glove box
Carry out.Whole technical process of the invention is all carried out in the anhydrous high-purity glove box of anaerobic, therefore beryllium powder oxygen impurities content is low.
It is further preferred that high purity inert gas oxygen content≤10ppm, water content≤1ppm in the glove box.
Further it is further preferred that the high purity inert gas are argon gas or nitrogen, preferably described high-purity indifferent gas
Purity >=99.999% of body.
The second object of the present invention, is the preparation facilities for providing the nanometer beryllium powder that a kind of above-mentioned method is used, and is adopted
Technical scheme is：Including source bottle, reaction bulb, bubbling bottle and condensing unit, the source bottle is anti-with described by the first pipeline
Bottle is answered to connect, the first pipeline periphery is provided with first heater, the source bottle is also connected with an air inlet pipe, the source bottle
It is placed in secondary heating mechanism, the reaction bulb is also connected with the condensing unit, the other end of the condensing unit is by the
Two pipelines are connected with the bubbling bottle, and the bubbling bottle is also associated with tail gas discharging pipe.
As preferred technical scheme, flow controller is provided with the air inlet pipe, and in the flow controller
Two ends are respectively arranged with valve.
As preferred technical scheme, valve is also equipped with the second pipe.
Used as preferred technical scheme, the first heater is heating tube.
Used as preferred technical scheme, the secondary heating mechanism is oil bath heating device.
As preferred technical scheme.Electronic thermometer is additionally provided with the reaction bulb.
Compared with prior art, the advantage of the invention is that：Relative to microlayer model sampling system, the beryllium powder particles diameter for obtaining
Thinner, its diameter is less than 65nm；The temperature that organic beryllium etherate of molecular state is pyrolyzed in mineral oil is homogeneous, incomplete decomposing ratio
Rate is small, and carbon impurity content is low, and carbon impurity content is less than 0.2at%；Whole technical process of the invention is all in the anhydrous height of anaerobic
Carried out in pure glove box, therefore beryllium powder oxygen impurities content is low；The present invention less, draws during preparing beryllium powder in the absence of transfer, contact
Enter that impurity is few, as the mineral oil solvent of pyrolysis heat transfer medium using after distilation, ICP-MS does not detect impurity, finally
The beryllium flour gold for obtaining belongs to total impurities less than 12ppm.
Brief description of the drawings
The structural representation of the preparation facilities that Fig. 1 is used by the embodiment of the present invention 1；
In figure：1 air inlet pipe, 2 first valves, 3 flow controllers, 4 second valves, 5 oil bath cylinders, 6 n-dodecanes, 7 is organic
Beryllium etherate, 8 n-dodecanes, 9 bubbling bottles, 10 n-dodecanes, 11 tail gas discharging pipes, 12 the 3rd valves, 13 second pipes, 14 magnetic
Power electric jacket, 15 three-neck flasks, 16 condenser pipes, 17 refrigerant outlets, 18 refrigerant inlets, 19 stainless steel pipes, 20 heating tubes,
21 electronic thermometers, 22 the 4th valves, 23 organic beryllium source bottles.
Specific embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1：
Overall process prepared by the beryllium powder of the present embodiment is carried out all in glove box.Atmosphere is high-purity argon gas in glove box
(99.999%), oxygen content≤10ppm, water content≤1ppm.Beryllium dust has high toxicity, therefore the experiment need to be prevented possessing beryllium
The specialized laboratories of guard strip part are carried out, and the tail gas that preparation process is produced enters air after reaching discharge standard through filtering, into experiment
Need to wear solid before room to test protective garment, wear protection half face shield, emgloves need to be worn during operation.
Referring to Fig. 1, concretely comprise the following steps：
1. solvent purifications：
The present embodiment uses n-dodecane (Aladdin reagent, purity 99%, CAS：112-53-8, boiling point is 217 DEG C) make
It is the heat transfer medium of pyrolysis；Before Pyrolysis Experiment, using distillation purifying n-dodecane, non-volatile impurities are removed；Vacuum distillation,
About 120 DEG C of n-dodecane fluid temperature, about 80 DEG C of steam temperature；N-dodecane after distillation analyzes display using ICP-MS, does not have
Detect metal impurities；
2. electron temperature meter calibrating：
Purified n-dodecane is added to three neck reaction flasks 15, by n-dodecane boiling steady temperature (217
DEG C) calibration electronic thermometer 21；
3. solvent heated constant temperature：
N-dodecane temperature is dropped to 200 DEG C, and remains constant；
4. Di-tert-butyl beryllium etherate steam pyrolytic reaction：
Di-tert-butyl beryllium etherate is added into organic beryllium source bottle 23, and by oil bath 5 by temperature control at 25 DEG C, this
When Di-tert-butyl beryllium etherate saturated vapour pressure about 35Torr-40Torr, about 5kpa, Di-tert-butyl beryllium second under poised state
Ether complex vapor concentration is about 5%；The first valve 2, the second invention 4, the 3rd valve 12 and the 4th valve 22 are opened, using super
Straight argon (99.9999%) is imported as carrier gas from air inlet pipe 1, and by flow controller 3, flow is controlled to 1slm, ultrapure argon
The bubbling in organic beryllium source bottle 23, (volume ratio is about for the mixed gas of formation argon gas-Di-tert-butyl beryllium etherate steam
19：1), by stainless steel pipes 19 (by the heating and thermal insulation of heating tube 20 at 25 DEG C) to three-neck flask 15, Di-tert-butyl beryllium ether
Complex gaseous molecular enters constant temperature, and in 200 DEG C of n-dodecane 8, there is pyrolytic reaction in moment, generation white
BeH2Powder, suspension is formed in n-dodecane 8；The reaction is the endothermic reaction, should be stirred rapidly, keeps the temperature of n-dodecane 8
It is homogeneous；
5.BeH2Decompose
Remain stirring, it is to avoid particle agglomeration, keep suspended liquid status；Solvent temperature is slowly raised 215 DEG C,
BeH28 decompose dehydrogenation, white BeH in n-dodecane2The slowly varying Be suspension into black of suspension.
6. separated solvent and drying
By separated n-dodecane solvent, beryllium powder is obtained：Temperature sensing point is positive 12 in reaction bulb in this step
Alkane steam, temperature control is at 90 DEG C or so.After distillation terminates, continue to vacuumize, heat, solvent is extracted in a gaseous form, directly
Dried completely to beryllium powder, temperature sensing point is n-dodecane steam in reaction bulb in the step, and temperature control is at 90 DEG C or so.
Dry beryllium powder is taken out from three-neck flask 15.
Embodiment 2
Using n-tridecane as pyrolysis heat transfer medium, other are same as Example 1.
Embodiment 3
Using n-tetradecane as pyrolysis heat transfer medium, other are same as Example 1.
Embodiment 4
Pyrolysis temperature is 230 DEG C, and other are same as Example 1.
Embodiment 5
Using glucinum ethyl etherate as raw material, other are same as Example 1.
The proterties testing result of the beryllium powder obtained by the embodiment 1-5 of embodiment 6：
Diameter, carbon impurity content, the metal impurities total content of the beryllium powder obtained by embodiment 1-5 are detected respectively, and its result is shown in
Table 1
The proterties testing result of the embodiment 1-5 of table 1 gained beryllium powder
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of nanometer of preparation method of beryllium powder, it is characterised in that：Comprise the following steps：
A () heats and constant temperature mineral oil；
B organic beryllium etherate steam is pipelined to step by () using carrier gas from source bottle（a）Heated constant temperature ore deposit
In thing oil；
C () organic beryllium etherate gaseous molecular is pyrolyzed generation BeH in mineral oil2, accessory substance isobutene, ether are arranged as tail gas
Go out；
(d) in mineral oil, BeH2The dehydrogenation of reheating solution generates beryllium；
E () separates mineral oil, and be dried to obtain a nanometer beryllium powder.
2. the according to claim 1 nanometer of preparation method of beryllium powder, it is characterised in that：The mineral oil be n-dodecane or
N-tridecane or n-tetradecane.
3. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that：Step（a）Heated constant temperature to 200 DEG C-
250 ℃。
4. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that：Organic beryllium etherate is diethyl
Beryllium etherate, Di-tert-butyl beryllium etherate.
5. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that：Step（b）The carrier gas is ultrapure argon
Or superpure nitrogen, purity >=99.9999 % of preferably described ultrapure argon or superpure nitrogen.
6. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that：Step（b）The carrier gas flux is
0.01 slm-5 slm。
7. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that：To step（b）The source bottle and pipeline
Heated, and the temperature of pipeline heating is consistent with the temperature of source bottle heating, the heating-up temperature of preferably described source bottle and pipeline
It is 20 DEG C -50 DEG C.
8. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that：The preparation process of methods described is in hand
Carried out in the middle and high pure inert gas environment of casing, high purity inert gas oxygen content≤10 ppm in preferably described glove box, water contains
≤ 1 ppm of amount；The further preferred high purity inert gas are argon gas or nitrogen, the purity of preferably described high purity inert gas >=
99.999 %。
9. the preparation facilities of the nanometer beryllium powder that the method for claim 1-8 any one is used, it is characterised in that including source
Bottle, reaction bulb, bubbling bottle and condensing unit, the source bottle are connected by the first pipeline with the reaction bulb, first pipeline
Periphery is provided with first heater, and the source bottle is also connected with an air inlet pipe, and the source bottle is placed in secondary heating mechanism, institute
State reaction bulb also to be connected with the condensing unit, the other end of the condensing unit is connected by second pipe with the bubbling bottle
Logical, the bubbling bottle is also associated with tail gas discharging pipe.
10. the according to claim 9 nanometer of preparation facilities of beryllium powder, it is characterised in that：Stream is provided with the air inlet pipe
Amount controller, and it is respectively arranged with valve at the two ends of the flow controller；Valve is also equipped with the second pipe；Institute
First heater is stated for heating tube；The secondary heating mechanism is oil bath heating device；Electricity is additionally provided with the reaction bulb
Sub- thermometer.
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|---|---|---|---|---|
| US3743710A (en) * | 1965-06-07 | 1973-07-03 | Ethyl Corp | Preparation of beryllium hydride |
| US3808063A (en) * | 1968-08-21 | 1974-04-30 | Ethyl Corp | Preparation of high density beryllium hydride |
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