CN106694905B - The preparation method and preparation facilities of a kind of nanometer of beryllium powder - Google Patents
The preparation method and preparation facilities of a kind of nanometer of beryllium powder Download PDFInfo
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- CN106694905B CN106694905B CN201710123461.1A CN201710123461A CN106694905B CN 106694905 B CN106694905 B CN 106694905B CN 201710123461 A CN201710123461 A CN 201710123461A CN 106694905 B CN106694905 B CN 106694905B
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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
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- 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 the preparation methods and preparation facilities of a kind of nanometer of beryllium powder, belong to beryllium powder preparation technical field, the method for use are as follows: are pipelined to organic beryllium etherate steam in the mineral oil of heated constant temperature from source bottle using carrier gas；Organic beryllium etherate gaseous molecular is pyrolyzed in mineral oil generates BeH2, by-product isobutene, ether are discharged as tail gas；In mineral oil, BeH2Reheating solution dehydrogenation generates beryllium；Separate mineral oil, and it is dried to obtain a nanometer beryllium powder, preparation facilities of the invention includes source bottle, reaction flask, bubbling bottle and condensing unit, the source bottle is connect with the reaction flask, the source bottle is also connected to an air inlet pipe, the reaction flask is also connected to the condensing unit, and the other end of the condensing unit is connected to by second pipe with the bubbling bottle；The beryllium powder that the present invention is prepared, diameter is smaller, less than 65 nm；Carbon impurity content is low, is lower than 0.2 at%, finally obtained beryllium flour gold category total impurities are less than 12 ppm.
Description
Technical field
The present invention relates to the preparation methods more particularly to a kind of organic beryllium etherate of use carrier gas carrying of a kind of nanometer of beryllium powder
The method that steam is pyrolyzed preparation nanometer beryllium powder into the mineral oil of heated constant temperature.
Background technique
Beryllium is a kind of rare light metals, has many special performances, is widely used in many important engineering fields, such as
Inertial navigation, optical system, guided missile, satellite, spacecraft and aviation etc..Metallic beryllium is substantially at present is obtained by powder metallurgy
, this is because beryllium ingot casting contains a large amount of hole, microscopic structure is coarse grain structure, even if after working process, crystal grain
Degree is also greater than 100 μm, and as a result the mechanical performance of beryllium ingot casting is excessively poor.Therefore the manufacture of beryllium part can only use powder metallurgic method, i.e.,
Beryllium ingot casting is turned into bits, powder is then made, is used further to subsequent working process.
With the development of science and technology, the especially appearance of a new generation's high intensity, high ductibility beryllium material, the preparation to beryllium powder
Propose tightened up requirement.The granularity of beryllium powder, chemical component, physical property, processing performance are to its consolidation process and final
Properties of product have great influence.Mechanical means is usually used in the preparation of beryllium powder, mainly has disc grinder, ball milling, impact to grind
Mill, gas atomization etc..The prevailing technology of beryllium powder production at present is impact grinding method, and obtained beryllium Powder Particle Size is in some tens of pm
Magnitude.This method is difficult to that the particle diameter of beryllium powder, and complex process equipment are greatly reduced again, at high cost, grinds repeatedly, the time
Long, often, powder temperature is high out, and degree of oxidation is high.It grinds equipment contact and introduces impurity.
Organic beryllium etherate is assigned in the mineral oil of heated constant temperature by present applicant using microlayer model generator
Pyrolysis has obtained nanometer beryllium powder, and 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 uses
The mode of microlayer model sample introduction, relatively natural drop, although microlayer model very little, be still by a large amount of organic beryllium molecules cohesions and
At the particle diameter of obtained beryllium powder is difficult to further decrease.Meanwhile there are temperature gradients 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 generates carbon compound, and carbon impurity is difficult to remove in beryllium powder, and in resulting beryllium powder, carbon impurity content is 1.5at% (atomicity
Percentage composition), higher carbon impurity content affects the quality and performance of beryllium powder, and metal impurities total amount is 20ppm or so.
Summary of the invention
An object of the present invention, in that the preparation method of a kind of nanometer of beryllium powder is provided, to solve the above problems.
To achieve the goals above, the technical solution adopted by the present invention is that it is such: the preparation method of a kind of nanometer of beryllium powder,
The following steps are included:
(a) by mineral oil heating and constant temperature；
(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 in mineral oil generates BeH2, by-product isobutene, ether are as tail
Gas discharge；
(d) in mineral oil, BeH2Reheating solution dehydrogenation generates beryllium；
(e) mineral oil is separated, and is dried to obtain a nanometer beryllium powder.
Organic beryllium etherate that the present invention realizes molecular state is pyrolyzed in mineral oil.
As a preferred technical scheme: the mineral oil is n-dodecane or n-tridecane or n-tetradecane.
As a preferred technical scheme: step (a) heated constant temperature is to 200 DEG C -250 DEG C.
As a preferred technical scheme: organic beryllium etherate is glucinum ethyl etherate, Di-tert-butyl beryllium second
Ether complex.
As a 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 a 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 a preferred technical scheme: step (b) source bottle and pipeline being heated, and the temperature of pipeline heating
Consistent with the temperature of source bottle heating, the heating temperature of the preferably described source bottle and pipeline is 20 DEG C -50 DEG C.
As a preferred technical scheme: the preparation process of the method is in the middle and high pure inert gas environment of glove box
It carries out.Entire technical process of the invention all carries 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 is argon gas or nitrogen, preferably described high-purity indifferent gas
Purity >=99.999% of body.
The second object of the present invention is to provide a kind of preparation facilities of nanometer beryllium powder used in above-mentioned method, adopt
Technical solution are as follows: including source bottle, reaction flask, bubbling bottle and condensing unit, source bottle passes through first pipe and described anti-
Bottle is answered to connect, the first pipe periphery is provided with first heater, and the source bottle is also connected to an air inlet pipe, the source bottle
It is placed in secondary heating mechanism, the reaction flask is also connected to the condensing unit, and the other end of the condensing unit passes through the
Two pipelines are connected to the bubbling bottle, and the bubbling bottle is also connected with tail gas discharging pipe.
Flow controller is provided in the air inlet pipe as a preferred technical solution, and in the flow controller
Both ends are respectively arranged with valve.
Valve is also equipped on the second pipe as a preferred technical solution,.
The first heater is heating tube as a preferred technical solution,.
The secondary heating mechanism is oil bath heating device as a preferred technical solution,.
As a preferred technical scheme.Electronic thermometer is additionally provided in the reaction flask.
Compared with the prior art, the advantages of the present invention are as follows: relative to microlayer model sampling system, obtained beryllium powder particles diameter
Thinner, diameter is lower than 65nm；The temperature that organic beryllium etherate of molecular state is pyrolyzed in mineral oil is uniform, incomplete decomposing ratio
Rate is small, and carbon impurity content is low, and carbon impurity content is lower than 0.2at%；Entire technical process of the invention is all in the anhydrous height of anaerobic
It is carried out in pure glove box, therefore beryllium powder oxygen impurities content is low；Transfer is not present during preparing beryllium powder in the present invention, and contact is few, draws
Enter that impurity is few, the mineral oil solvent as pyrolysis heat transfer medium is using after distilation, and ICP-MS does not detect impurity, finally
Obtained beryllium flour gold category total impurities are less than 12ppm.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of preparation facilities 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 third 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
The present invention will be further described with reference to the accompanying drawings.
Embodiment 1:
The overall process of the beryllium powder preparation of the present embodiment carries 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 having beryllium
The specialized laboratories of guard strip part carry out, and the tail gas that preparation process generates is discharged into atmosphere after filtering up to discharge standard, into experiment
It needs to wear solid before room to test protective garment, wears protection half face shield, when operation need to wear emgloves.
Referring to Fig. 1, specific steps are as follows:
1. solvent purifications:
The present embodiment is made using n-dodecane (Aladdin reagent, purity 99%, CAS:112-53-8, boiling point are 217 DEG C)
For 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 use ICP-MS analysis shows that, do not have
Detect metal impurities；
2. electron temperature meter calibrating:
Purified n-dodecane is added to three neck reaction flasks 15, passes through 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:
Organic beryllium source bottle 23 is added in Di-tert-butyl beryllium etherate, and is controlled temperature at 25 DEG C by oil bath 5, this
When Di-tert-butyl beryllium etherate saturated vapour pressure about 35Torr-40Torr, about 5kpa, Di-tert-butyl beryllium second under equilibrium state
Ether complex vapor concentration is about 5%；The first valve 2, the second invention 4, third valve 12 and the 4th valve 22 are opened, using super
Straight argon (99.9999%) is used as carrier gas, imports from air inlet pipe 1, by flow controller 3, flow control 1slm, ultrapure argon
It is bubbled in organic beryllium source bottle 23, forming argon gas-Di-tert-butyl beryllium etherate steam mixed gas, (volume ratio is about
19:1), three-neck flask 15, Di-tert-butyl beryllium ether are arrived by stainless steel pipes 19 (by 20 heating and thermal insulation of heating tube at 25 DEG C)
Complex gaseous molecular enters constant temperature, and in 200 DEG C of n-dodecane 8, pyrolytic reaction occurs for moment, generates white
BeH2Powder forms suspension in n-dodecane 8；The reaction is the endothermic reaction, should be stirred rapidly, and 8 temperature of n-dodecane is kept
It is uniform；
5.BeH2It decomposes
It remains stirring, avoids 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 at black of suspension.
6. distillation separation solvent and drying
Be separated by distillation n-dodecane solvent, obtain beryllium powder: temperature sensing point is positive 12 in reaction flask in this step
Alkane steam, temperature are controlled at 90 DEG C or so.After distillation, continue to vacuumize, heat, solvent is extracted in a gaseous form, directly
It is dried completely to beryllium powder, temperature sensing point is n-dodecane steam in reaction flask in the step, and temperature is controlled at 90 DEG C or so.
Dry beryllium powder is taken out from three-neck flask 15.
Embodiment 2
It is other same as Example 1 using n-tridecane as pyrolysis heat transfer medium.
Embodiment 3
It is other same as Example 1 using n-tetradecane as pyrolysis heat transfer medium.
Embodiment 4
Pyrolysis temperature is 230 DEG C, other same as Example 1.
Embodiment 5
It is other same as Example 1 using glucinum ethyl etherate as raw material.
The character testing result of the obtained beryllium powder of 6 embodiment 1-5 of embodiment:
Diameter, carbon impurity content, the metal impurities total content for detecting the resulting beryllium powder of embodiment 1-5 respectively, the result is shown in
Table 1
The character testing result of beryllium powder obtained by 1 embodiment 1-5 of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (15)
1. the preparation method of a kind of nanometer of beryllium powder, it is characterised in that: the following steps are included:
(a) by mineral oil heating and constant temperature；
(b) organic beryllium etherate steam is pipelined to the mine of the heated constant temperature of step (a) using carrier gas from source bottle
In object oil；
(c) organic beryllium etherate gaseous molecular is pyrolyzed in mineral oil generates BeH2, by-product isobutene, ether are arranged as tail gas
Out；
(d) in mineral oil, BeH2Reheating solution dehydrogenation generates beryllium；
(e) mineral oil is separated, and is dried to obtain a nanometer beryllium powder.
2. the preparation method of according to claim 1 nanometer 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) carrier gas is ultrapure argon
Or superpure nitrogen.
6. the preparation method of nanometer beryllium powder according to claim 5, it is characterised in that: the ultrapure argon or superpure nitrogen it is pure
Spend >=99.9999 %.
7. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that: step (b) carrier gas flux is
0.01 slm-5 slm。
8. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that: to step (b) source bottle and pipeline
It is heated, and the temperature of pipeline heating is consistent with the temperature of source bottle heating.
9. the preparation method of nanometer beryllium powder according to claim 8, it is characterised in that: the heating temperature of the source bottle and pipeline
It is 20 DEG C -50 DEG C.
10. the preparation method of nanometer beryllium powder according to claim 1, it is characterised in that: the preparation process of the method exists
It is carried out in the middle and high pure inert gas environment of glove box.
11. the preparation method of nanometer beryllium powder according to claim 10, it is characterised in that: high-purity inertia in the glove box
Gas oxygen content≤10 ppm, water content≤1 ppm.
12. the preparation method of nanometer beryllium powder according to claim 11, it is characterised in that: the high purity inert gas is argon gas
Or nitrogen.
13. the preparation method of nanometer beryllium powder according to claim 12, it is characterised in that: the high purity inert gas it is pure
Spend >=99.999 %.
14. the preparation facilities of nanometer beryllium powder used in the method for claim 1-13 any one, which is characterized in that including source
Bottle, reaction flask, bubbling bottle and condensing unit, the source bottle are connect by first pipe with the reaction flask, the first pipe
Periphery is provided with first heater, and the source bottle is also connected to an air inlet pipe, and the source bottle is placed in secondary heating mechanism, institute
It states reaction flask to be also connected to the condensing unit, the other end of the condensing unit is connected by second pipe and the bubbling bottle
Logical, the bubbling bottle is also connected with tail gas discharging pipe.
15. the preparation facilities of according to claim 14 nanometer of beryllium powder, it is characterised in that: be provided with stream in the air inlet pipe
Amount controller, and valve is respectively arranged at the both ends of the flow controller；Valve is also equipped on the second pipe；Institute
Stating first heater is heating tube；The secondary heating mechanism is oil bath heating device；Electricity is additionally provided in the reaction flask
Sub- thermometer.
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| US3816608A (en) * | 1967-10-05 | 1974-06-11 | Ethyl Corp | Preparation of beryllium hydride by pyrolysis of a di-tertiary-alkyl beryllium etherate |
| CN1144967A (en) * | 1995-09-04 | 1997-03-12 | 冶金工业部钢铁研究总院 | Manufacture method and device for metal magnetic liquid |
| CN103482571A (en) * | 2013-09-26 | 2014-01-01 | 中国工程物理研究院激光聚变研究中心 | Preparation method and device for beryllium hydride material |
| CN105728746A (en) * | 2016-05-11 | 2016-07-06 | 中国工程物理研究院激光聚变研究中心 | Preparing method of nano beryllium powder |
| CN206509522U (en) * | 2017-03-03 | 2017-09-22 | 中国工程物理研究院激光聚变研究中心 | A kind of preparation facilities of nanometer of beryllium powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3808063A (en) * | 1968-08-21 | 1974-04-30 | Ethyl Corp | Preparation of high density beryllium hydride |
| CN1056460C (en) * | 1998-04-29 | 2000-09-13 | 冶金工业部钢铁研究总院 | Method for making iron nitride magnetic fluid |
| CN1133584C (en) * | 1999-11-05 | 2004-01-07 | 刘庆昌 | Gas phase synthesis process of superfine titanium carbide powder |
| CN1590292A (en) * | 2004-06-10 | 2005-03-09 | 江南大学 | Chemical gas phase sedimentation preparation method of nano silicone dioxide |
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2017
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3743710A (en) * | 1965-06-07 | 1973-07-03 | Ethyl Corp | Preparation of beryllium hydride |
| US3816608A (en) * | 1967-10-05 | 1974-06-11 | Ethyl Corp | Preparation of beryllium hydride by pyrolysis of a di-tertiary-alkyl beryllium etherate |
| CN1144967A (en) * | 1995-09-04 | 1997-03-12 | 冶金工业部钢铁研究总院 | Manufacture method and device for metal magnetic liquid |
| CN103482571A (en) * | 2013-09-26 | 2014-01-01 | 中国工程物理研究院激光聚变研究中心 | Preparation method and device for beryllium hydride material |
| CN105728746A (en) * | 2016-05-11 | 2016-07-06 | 中国工程物理研究院激光聚变研究中心 | Preparing method of nano beryllium powder |
| CN206509522U (en) * | 2017-03-03 | 2017-09-22 | 中国工程物理研究院激光聚变研究中心 | A kind of preparation facilities of nanometer of beryllium powder |
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