CN103708419A - Method for preparing of high-activity LiH microspheres through wet process - Google Patents
Method for preparing of high-activity LiH microspheres through wet process Download PDFInfo
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- CN103708419A CN103708419A CN201310741088.8A CN201310741088A CN103708419A CN 103708419 A CN103708419 A CN 103708419A CN 201310741088 A CN201310741088 A CN 201310741088A CN 103708419 A CN103708419 A CN 103708419A
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- lithium hydride
- microballoon
- paraffin
- argon
- microspheres
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000004005 microsphere Substances 0.000 title claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910000103 lithium hydride Inorganic materials 0.000 claims abstract description 56
- 229910052786 argon Inorganic materials 0.000 claims abstract description 45
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000012188 paraffin wax Substances 0.000 claims abstract description 25
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 239000012047 saturated solution Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 claims abstract 17
- 239000007789 gas Substances 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 16
- 230000009257 reactivity Effects 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 3
- 239000011268 mixed slurry Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 235000011194 food seasoning agent Nutrition 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 12
- 238000000465 moulding Methods 0.000 abstract description 8
- 238000004512 die casting Methods 0.000 abstract description 4
- 238000011049 filling Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract 2
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 42
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 208000037656 Respiratory Sounds Diseases 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000011232 storage material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- -1 neutron moderator Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 206010011376 Crepitations Diseases 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011824 nuclear material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229910052722 tritium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
一种湿法制备高活性LiH微球的方法，属于陶瓷材料领域。完成步骤如下：（1）配制浆料：以石蜡溶解在石油醚或乙醚的饱和溶液作为球磨介质，在氩气气氛中球磨氢化锂得稳定、均匀的浆料；（2）成型微球坯体：在流通的氩气塔中滴落成球；（3）烧结：在气氛炉中通氩气烧结，以10℃每小时升温，分四段保温，在450℃烧结4小时，以30℃每小时降温；（4）微球包覆：烧结后的微球放入石蜡在石油醚或乙醚的过饱和溶液中，取出微球在氩气中干燥。该方法制备氢化锂微球具有大小均一、球形度高、机械性能好、微球直径可控等特点以外，还避免了熔融法制备氢化锂微球产生的大量裂纹以及热压铸成型充模和脱模难等问题，并且设备和制备工艺简单、效率高、能批量生产。
The invention discloses a wet method for preparing high-activity LiH microspheres, which belongs to the field of ceramic materials. The completion steps are as follows: (1) Prepare the slurry: use the saturated solution of paraffin dissolved in petroleum ether or ether as the ball milling medium, and ball mill lithium hydride in an argon atmosphere to obtain a stable and uniform slurry; (2) Form the microsphere green body : drop into balls in the circulating argon tower; (3) sintering: sintering in an atmosphere furnace with argon, heating up at 10°C per hour, keeping it in four sections, sintering at 450°C for 4 hours, and sintering at 30°C per hour Cool down; (4) microsphere coating: put the sintered microspheres into a supersaturated solution of paraffin in petroleum ether or ether, take out the microspheres and dry them in argon. The preparation of lithium hydride microspheres by this method has the characteristics of uniform size, high sphericity, good mechanical properties, and controllable diameter of the microspheres. It also avoids a large number of cracks produced by the melting method of lithium hydride microspheres and hot die-casting molding filling and stripping. Difficult molds and other problems, and the equipment and preparation process are simple, efficient, and can be mass-produced.
Description
Technical field
The invention belongs to stupalith field, relate to the preparation method of ceramic microsphere, particularly a kind of the preparation of high reactivity LiH microballoon wet method and method for coating for nuclear fusion stack tritium propagation ceramic microsphere and hydrogen storage material field.
Background technology
Lithium hydride (LiH) has in vacuum and inert atmosphere that ordination number is little, thermodynamics is relatively stable, mechanical property is excellent, fusing point high (688 ℃), the low (0.775g/cm of density
3), hydrogeneous and high by (5.82 * 10 containing lithium amount
22atoms/cm
3) etc. excellent performance.This stupalith can be used as structure and function material and is widely used in new energy materials field.As nuclear energy field can be used as neutron shielding material, neutron moderator, ceramic tritium-breeding material, ICF target materials etc.; In hydrogen storage material field, because hydrogen density surpasses liquid hydrogen, can be used as the solid-state hydrogen storage material of excellent performance.Lithium hydride microballoon have handling easily, transportation is convenient, specific surface area is large, the diffusion of gas and release property is good, to be conducive to thermal stresses lax and prevent the excellent properties such as irradiation cracking.Therefore, generally all need lithium hydride to be prepared into microballoon.
Lithium hydride is because chemical property is very active, can with most substance reactions, produce hydrogen and corresponding lithium-containing compound.Powder lithium hydride can spontaneous combustion in damp atmosphere, the reaction of blasting in the nitrogen of heating.Therefore the preparation of the microballoon of lithium hydride is very difficult.In the 1950's, the U.S. and Soviet Union material supply section scholar using lithium hydride as Nuclear weapons and space power source done widely research, comprising the preparation of microballoon.Owing to relating to military secret, all Research Literatures are just open in decades recently.But all do not obtain and be satisfied with achievement through a lot of experiments.Document 1(H. Sheinberg, R.E. Riley and J.M. Taub, Los Alamos Scientific Laboratory Report no. LA-4905-MS (April 1972)) be reported in metal hydride simple substance lithium in oil bath, but only seldom part success, and efficiency is low, sphericity is bad.Document 2(C.E. Messer, A Survey on Lithium Hydride, US AEC Report no. NYO-9470 (Oct. 1970)) in, adopt molten atomizing legal system for lithium hydride microballoon, but because of have an appointment when solidifying 19% volumetric shrinkage of lithium hydride, there is a large amount of crackles on the inner and surface of the microballoon of preparing and failure.(Carstens D H W, Farnum E H, Fries R J, et al. Fabrication of LiD in document 3
0.5t
0.5microspheres for use as laser fusion targets [J]. Journal of Nuclear Materials, 1975,57 (1): 1-10) adopt granulation scorification to prepare (40-125 μ m) microballoon performance and be relatively good, but spherome surface crackle is many, ultimate compression strength is little, and efficiency is low and involve great expense.
summary of the invention
The present invention will solve key issue, change scorification and prepare lithium hydride microballoon present situation, avoid cracking because comparatively large vol shrinks, also avoid the problem such as mold filling and demoulding difficulty in hot die-casting molding simultaneously, reduce and prepare lithium hydride microballoon cost of equipment, and can manufacture out good sphericity, mechanical property is excellent, the lithium hydride microballoon that density is high, and for convenience of storing and transporting, lithium hydride microballoon is coated to processing.
Technical scheme of the present invention is:
Wet method is prepared the method for high reactivity LiH microballoon:
(1) preparation of slurry: take solid paraffin and sherwood oil or ether as raw material, under room temperature, solid paraffin is dissolved in sherwood oil or ether, be made into the saturated solution of paraffin, again in the glove box of argon gas atmosphere lithium hydride block and paraffin saturated solution by volume 1:1 put into vacuum sphere grinding jar, add again appropriate steel ball, after vacuumizing, in an atmospheric argon gas, ball milling is 4 ~ 8 hours, forms stable, uniform lithium hydride slurry;
(2) moulding of microballoon: the slurry after ball milling in above-mentioned steps (1) is completed to moulding and dry in Fig. 1 device simultaneously.First closing switch 1 and material are managed switch 9, open tracheae switch 7, open vacuum pump 6, sealed vessel 3 is vacuumized, then from airway 5, be filled with argon gas, making sealed vessel 3 internal pressures is a normal atmosphere, realize argon shield slurry, then open switch 1, from feed-pipe 2, add the slurry after ball milling in above-mentioned steps (1), open the abundant mixed slurry of agitator 4, then open recovery catheter switch 21 and tunger tube switch 18 simultaneously and pass into argon gas, regulate argon gas pump 17, making argon flow amount in argon air tower 12 is 200 milliliters of per minutes, displace the air in argon air tower, open again material pipe switch 9, regulate pump and under meter 10, the speed that makes dropper 13 ooze microballoon 14 be 2 seconds each, the argon gas flowing out from gas mesh sieve 15 makes microballoon 14 slow decreasings, and the argon gas of circulation is taken away sherwood oil or the ether in microballoon 14, microballoon 14 is dried.Select different diameter dropper 13, the titratable microballoon that goes out different diameter;
(3) sintering: the dried microballoon that above-mentioned steps (2) is oozed, logical argon gas sintering in atmosphere furnace, temperature rise rate be 10 ℃ per hour, 55 ℃ of insulations 30 minutes, at 230 ℃, 350 ℃ and 410 ℃, be incubated respectively 60 minutes, 450 ℃ of sintering 4 hours, with 30 ℃, per hourly cool to 200 ℃ subsequently, then cool to room temperature with stove;
(4) microballoon is coated: the microballoon after above-mentioned steps (3) sintering is put into the sherwood oil of paraffin or the supersaturated solution of ether, then it is dry in argon gas atmosphere glove box to take out lithium hydride microballoon, and after sherwood oil or ether volatilization, the completely coated microballoon of paraffin.
The present invention compared with prior art had advantages of:
(1) technical process of the present invention is simple, easy to operate, efficiency is high, can manufacture, and has reduced the high cost of equipment that scorification is prepared lithium hydride microballoon;
(2) microballoon good sphericity, big or small homogeneous, good mechanical property, and surface and inside do not have crackle, avoided scorification to prepare the crackle of lithium hydride generation;
(3) after green microspheres is dried, paraffin is wrapping lithium hydride fine powder, has completely cut off lithium hydride and has contacted with external substance, has prevented the oxidation of lithium hydride;
(4) to the lithium hydride microballoon after sintering, carried out paraffin coated, facilitated transportation and the storage of lithium hydride microballoon, and coating layer easily removes, in sherwood oil that only need be after intensification or ether, washing just can be removed paraffin coating layer several times;
(5) compare with hot die-casting molding, only adopting sherwood oil or ether is that the paraffin saturated solution of solvent is as lithium hydride ball-milling medium, lithium hydride green microspheres paraffinicity is low, and lithium hydride solid content is high, has avoided the problems such as mold filling in hot die-casting molding, demoulding difficulty simultaneously.
Accompanying drawing explanation
Fig. 1 be the present invention design prepare the moulding of lithium hydride green microspheres and dry schematic diagram.
In figure: 1 switch, 2 feed conduits, 3 sealed vessels, 4 agitators, 5 airways, 6 vacuum pumps, 7 tracheae switches, 8 sealing baffles, 9 material pipe switches, 10 pumps and under meter, 11 material pipes, 12 argon air towers, 13 droppers, 14 microballoons, 15 gas mesh sieves, 16 tunger tubes, 17 argon gas pumps, 18 tunger tube switches, 19 argon gas, 20 reclaim conduit, 21 and reclaim catheter switch.
Fig. 2 is the X ray diffracting spectrum (XRD) that the embodiment of the present invention 1 is prepared lithium hydride microballoon.
Detected result shows, as technological invention content, the lithium hydride microballoon sphericity that wet method is prepared and density is high, surface and inside do not have crackle, and acquisition for microballoon be pure lithium hydride.
embodiment:
embodiment 1:
(1), under room temperature, 10 grams of paraffin are dissolved in the sherwood oil of 30 milliliters.After dissolution equilibrium, get supernatant liquid, obtain the saturated solution of paraffin;
(2) saturated solution of pressing in lithium hydride and above-mentioned steps (1) is long-pending than 1:1, takes 15 grams of lithium hydrides, 13.6 grams of paraffin saturated solutions, suitably grain size proportion steel ball, is positioned over vacuum sphere grinding jar, after vacuumizing, in ball grinder, be filled with an atmospheric argon gas, ball milling 6 hours;
(3) at argon gas gloves, take out the slurry after above-mentioned steps (2) ball milling in mutually, adopt the moulding of Fig. 1 device.First closing switch 1 and material are managed switch 9, open tracheae switch 7, open vacuum pump 6, sealed vessel 3 is vacuumized, then from airway 5, be filled with argon gas, making sealed vessel 3 internal pressures is a normal atmosphere, realize argon gas atmosphere protective paste, then open switch 1, from feed-pipe 2, add the slurry after ball milling in above-mentioned steps (2), open the abundant mixed slurry of agitator 4, then open simultaneously reclaim catheter switch 21 and tunger tube switch 18, regulate argon gas pump 17, making argon flow amount in argon air tower 12 is 200 milliliters of per minutes, displace the air in argon air tower, open again material pipe switch 9, regulate pump and under meter 10, the speed that makes dropper 13 ooze microballoon 14 be 2 seconds each, the argon gas flowing out from gas mesh sieve 15 makes microballoon 14 slow decreasings, and the argon gas of circulation is taken away the sherwood oil in microballoon 14, make microballoon 14 dry,
(4) collect dry rear microballoon in above-mentioned steps (3), in atmosphere furnace, logical argon gas sintering.Argon gas flow velocity is 80 milliliters of per minutes, temperature rise rate be 10 ℃ per hour, 55 ℃ of insulations 30 minutes, at 230 ℃, 350 ℃ and 410 ℃, be incubated respectively 60 minutes, 450 ℃ of sintering 4 hours, with 30 ℃, per hourly cool to 200 ℃ subsequently, with stove, cool to room temperature, obtaining the lithium hydride microballoon of 1 millimeter.Microballoon X-ray diffractogram (XRD) is as Fig. 2;
(5) the lithium hydride microballoon after above-mentioned steps (4) sintering is positioned in the paraffin supersaturated solution of 40 ℃, then homodisperse taking-up, is positioned over seasoning in argon gas, obtains the coated lithium hydride microballoon of paraffin.
embodiment 2:
Sherwood oil in embodiment 1 makes ether into, and all the other parameters are identical.
Claims (4)
1. wet method is prepared a method for high reactivity LiH microballoon, it is characterized in that the step of preparation is:
(1), adopt the saturated solution of paraffin in sherwood oil or ether as lithium hydride the ball-milling medium in argon gas;
(2), only adopt in saturated solution paraffin as the forming skeleton material of lithium hydride green microspheres in argon air tower;
(3), adopt the supersaturated solution of paraffin as the coating material of lithium hydride microballoon.
2. wet method according to claim 1 is prepared the method for high reactivity LiH microballoon, it is characterized in that:
In described step (1), in argon gas atmosphere during ball milling, the volume ratio 1:1 of paraffin saturated solution and lithium hydride; Concrete grammar is as follows:
At room temperature configuring the saturated solution of paraffin in sherwood oil or ether, is that 1:1 takes raw material by the volume ratio of saturated solution and lithium hydride, puts into vacuum sphere grinding jar, and after vacuumizing, in an atmospheric argon gas atmosphere, ball milling is 4 ~ 8 hours.
3. wet method according to claim 1 is prepared the method for high reactivity LiH microballoon, it is characterized in that:
In described step (2), in argon air tower, paraffin is as the framework material of lithium hydride green microspheres, and wherein in argon air tower, the flow velocity of argon gas is 200 milliliters of per minutes; Concrete grammar is as follows:
First closing switch (1) and material are managed switch (9), open tracheae switch (7), open vacuum pump (6), sealed vessel (3) is vacuumized, then from airway (5), be filled with argon gas, sealed vessel (3) internal pressure is a normal atmosphere; Then open switch (1), from feed-pipe (2), add ball milling disposed slurry, open agitator (4) mixed slurry, then open recovery catheter switch (21) and tunger tube switch (18) simultaneously and pass into argon gas, regulate argon gas pump (17), in argon air tower (12), argon flow amount is 200 milliliters of per minutes, then opens material pipe switch (9), regulate pump and under meter (10), the speed that dropper (13) oozes microballoon (14) be 2 seconds each.
4. wet method according to claim 1 is prepared the method method of high reactivity LiH microballoon, it is characterized in that:
In described step (3), use the supersaturated solution of paraffin as the coated raw material of lithium hydride microballoon, concrete grammar is as follows:
Lithium hydride microballoon is put into the supersaturated solution of paraffin, then taken out the argon gas glove box seasoning that lithium hydride microballoon is put into room temperature.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104393267A (en) * | 2014-10-24 | 2015-03-04 | 上海四驱新能源科技有限公司 | Preparation method of high-stability lithium metal microsphere powder |
| CN107225252A (en) * | 2017-07-25 | 2017-10-03 | 天津中能锂业有限公司 | A kind of passivation of lithium microballoon production method |
| CN112607706A (en) * | 2020-12-04 | 2021-04-06 | 中核建中核燃料元件有限公司 | Method for reducing activity of high-activity lithium hydride powder |
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- 2013-12-27 CN CN201310741088.8A patent/CN103708419B/en not_active Expired - Fee Related
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104393267A (en) * | 2014-10-24 | 2015-03-04 | 上海四驱新能源科技有限公司 | Preparation method of high-stability lithium metal microsphere powder |
| CN107225252A (en) * | 2017-07-25 | 2017-10-03 | 天津中能锂业有限公司 | A kind of passivation of lithium microballoon production method |
| CN112607706A (en) * | 2020-12-04 | 2021-04-06 | 中核建中核燃料元件有限公司 | Method for reducing activity of high-activity lithium hydride powder |
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