CN105110792A - Ball milling preparation method for high-uniformity YAG transparent ceramic powder - Google Patents
Ball milling preparation method for high-uniformity YAG transparent ceramic powder Download PDFInfo
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Abstract
The invention relates to a ball milling preparation method for YAG transparent ceramic powder used in a procedure of preparation for a YAG transparent ceramic, and belongs to the technical field of transparent ceramic preparation. The method comprises four key detailed processes of ball milling, shaking, sieving and secondary ball milling on slurry. Compared with a common ball milling preparation method, in which only one conventional ball milling procedure is carried out, for the YAG transparent ceramic powder, the delicate and high-operability ball milling preparation method provided by the invention is added with the step of shaking of a ball milling tank up and down in the preparation process, so that raw material powder deposited at the upper part of the ball milling tank can be shaken and sufficiently mixed through ball milling in the subsequent ball milling process; the sieving step is added, so that raw material agglomerated hard particles which are hard to be broken through ball milling can be effectively removed; the ball milling preparation method provided by the invention is further added with the step of secondary ball milling on the slurry, so that the raw material powder can be fully broken and mixed again, and adverse effects on powder uniformity caused by powder deposited at a joint of the ball milling tank and a ball milling tank lid as well as powder deposited at the top of the ball milling tank can be reduced.
Description
Technical field
The present invention relates to the preparation method of YAG crystalline ceramics, be specifically related to the ball-milling technology method preparing one of YAG crystalline ceramics committed step, mainly comprise ball milling, rock, sieve and slurry secondary ball milling four steps, belong to crystalline ceramics preparing technical field.
Technical background
Compared with monocrystalline, laser transparent ceramic material has three large significant advantages: (1) can realize high-concentration dopant and the grade doping of active ions, (2) have higher shaking property of heat resistanceheat resistant and breaking tenacity, (3) can prepare the optical module of large size and special shape; In addition, transparent laser ceramic also has that sintering temperature is low, preparation cycle is short, cost is low and the advantage such as quality controllability is strong.(Ikesue, the A. such as nineteen ninety-five Japanese Scientists Ikesue; Kinoshita, T.; Kamata, K.; Yoshida, K.Fabricationandopticalpropertiesofhigh-performancepolyc rystallineNd:YAGceramicsforsolid-statelasers.Journalofth eAmericanCeramicSociety.1995,78,1033 – 1040) scatter loss is low reaches 0.009cm to adopt solid reaction process to prepare
-1nd:YAG laser transparent ceramic, the measuring result of the physical propertys such as its specific refractory power, thermal conductivity, hardness shows, Nd:YAG laser transparent ceramic and Nd:YAG monocrystalline similar, have developed the transparent ceramic laser that First is laser diode-pumped in the world, its slope efficiency reaches 28% simultaneously.Since then, laser transparent ceramic material research is obtained extensive attention, and Japan, the U.S., France, Russia, Singapore, Korea S and China carry out laser transparent ceramic research one after another.Large-sized laser transparent ceramic is the material foundation of development high energy and power laser apparatus.
The processing step adopting solid reaction process to prepare YAG crystalline ceramics generally comprises: (1) prepares burden by component design; (2) by design speed and time, with ball mill ball milling raw material; (3) discharging, dry, sieve; (4) by stainless steel mould compression molding; (5) by design sintering process program vacuum high-temperature sintering; Anneal in (6) 1400 ~ 1500 DEG C of air; (7) the meticulous polishing of Single-handed Dinghy open-Laser.The quality that these steps complete all can have an impact to final laser transparent ceramic quality.In YAG crystalline ceramics, the appearance of dephasign can cause serious scatter loss, and therefore the formulating of recipe of YAG crystalline ceramics is all according to the chemical formula Y of YAG
3al
5o
12calculate raw material Y
2o
3and Al
2o
3content, simultaneously in order to acceleration of sintering, the sintering aid MgO and tetraethoxy (SiO that add trace need be combined
2), so the difficult point adopting solid phase method to prepare YAG crystalline ceramics does not lie in the exploration of formula, and be the research of fabricating technology, wherein just comprise ball-milling technology step.Such as, the people (LiuJun such as LiuJun; LinLi; LiJiang; LiuJing; YuanYong; IvanovMaxim; ChenMin; LiuBinglong; GeLin; XieTengfei; KouHuamin; ShiYun; PanYubai; GuoJingkun.Effectsofballmillingtimeonmicrostructureevolu tionandopticaltransparencyofNd:YAGceramics.CeramicsInter national.2014,40 (7), 9841-9851.)) just have studied the Microstructure evolution of Ball-milling Time on Nd:YAG crystalline ceramics and the impact of optical transmittance.But, about in the Research Literature of YAG crystalline ceramics or patent, for the description of ball-milling technology step, all only also be only limitted to crucial Ball-milling Time, the ratio of abrading-ball/YAG raw material/ball-milling medium, and rotational speed of ball-mill, and it is meticulousr all not introduce in actual mechanical milling process, workable concrete grammar step, the scientific worker carrying out crystalline ceramics research knows only according to the key parameter of these reports, be difficult to repeat to prepare high-quality YAG crystalline ceramics, and the mechanical milling process deliberate steps played an important role is only the emphasis exploratory development content of YAG crystalline ceramics technology of preparing.The mechanical milling process of YAG crystalline ceramics needs to reach simultaneously pulverizes feed particles and the even object of batch mixing.But prepare Y in factory
2o
3or Al
2o
3in material powder process, need through calcination process, Y
2o
3or Al
2o
3more or less can there is the reunion grit, particularly Al that are difficult on a small quantity rely on ball mill pulverizing in material powder
2o
3the probability that in material powder, this reunion grit exists is larger.In addition, at the seam crossing of ball grinder and ball milling cover, or also there will be the deposition of powder at the top (vertical-type planetary ball mill) of ball grinder, the powder of this part deposition cannot be mixed by abundant ball milling, and the homogeneity of ball milling powder finally can be caused to reduce.If can not effectively pulverize or isolate those reunion grits in mechanical milling process, and make material powder reach the mixing of sufficient ball milling, the YAG ceramic powder homogeneity so prepared through ball milling will reduce greatly, these reunion grits enter into YAG ceramic body with the material powder with component segregation, macrosegregation dephasign will be formed through oversintering, cause serious scatter loss.
In sum, YAG crystalline ceramics belongs to meticulous function ceramics field, and require very high to technology of preparing, carrying out the ball-milling technology technique study of details more, is vital to preparing high-property YAG crystalline ceramics.The invention provides a set of meticulous, workable YAG ceramic powder ball-milling preparation method, effectively can improve YAG transparent ceramic powder homogeneity, establishing powder basis for preparing high-quality YAG crystalline ceramics.
Summary of the invention
[technical problem that will solve]
The object of the invention is to obtain meticulous, workable YAG crystalline ceramics ball-milling preparation method, improving YAG transparent ceramic powder homogeneity, establishing powder basis for preparing high-quality YAG crystalline ceramics.
[technical scheme]
In order to reach above-mentioned technique effect, the present invention takes following technical scheme to realize:
Meticulous, a workable height even YAG transparent ceramic powder ball-milling preparation method, it is characterized in that comprising ball milling, rock, sieve and slurry secondary ball milling four Key detail processes, its concrete steps are as follows:
Step (1): according to the YAG crystalline ceramics formula of design, by Al
2o
3, Y
2o
3, tetraethoxy and nano-MgO put into the ball grinder that aluminum oxide abrading-ball is housed successively after weighing, and then pours alcohol into;
Step (2): will be fixed on planetary ball mill through step (1) charged ball grinder with the rotating speed ball milling 3 ~ 6 hours of 220 ~ 250r/min; Then taken off by ball grinder, do not take off lid dandle 5 ~ 10 times, object is the deposition material powder being attached to ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder rocked is fixed on planetary ball mill again, continues ball milling 3 ~ 6 hours according to the revolution of milling parameters 220 ~ 250r/min;
Step (3): the slurry after step (2) ball milling is poured in 200 ~ 400 object nylon mesh and sieves, object is to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further;
Step (4): in order to reduce the deposition of powder at the seam crossing of ball grinder and ball milling cover to the disadvantageous effect of powder homogeneity, the slurry obtained sieving through step (3) pour into again clean fill in the ball grinder of aluminum oxide abrading-ball, continue ball milling 3 ~ 6 hours according to the rotating speed of milling parameters 160 ~ 220r/min; Then taken off by ball grinder, do not take off and cover again dandle 5 ~ 10 times, object is to be continued by the material powder being deposited on ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder shaken is fixed on planetary ball mill again, continues ball milling 3 ~ 6 hours according to the revolution of milling parameters 160 ~ 220r/min;
Step (5): the slurry after step (4) ball milling is poured in 400 ~ 600 object nylon mesh and sieves, object is again to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further; The slurry this time obtained is the slurry after final ball milling, is passed through oven dry, namely sieve prepares the even YAG transparent ceramic powder of described height.
The present invention is technical scheme further, in step (1), and described Al
2o
3, Y
2o
3, the total mass of tetraethoxy and nano-MgO, aluminum oxide mill ball quality and alcohol mass ratio be 1:5.7:1.6 ~ 1.8.
The present invention is technical scheme further, and the rotational speed of ball-mill of described step (2) is greater than the rotational speed of ball-mill of described step (4).
The present invention is technical scheme further, and the nylon grit number of described step (3) is less than the nylon grit number of described step (5).
The present invention will be explained below.
In first time mechanical milling process, the object of not taking off lid dandle is rocked evenly by the deposition material powder being attached to ball grinder top, then continuation with during same rotational speed ball milling by abundant ball milling; Then sieve, to remove the reunion grit that cannot rely on ball mill crushing in raw material, improve the homogeneity of ball milling material powder further; Then the second time ball milling of slurry is carried out, can fully broken and blend feedstock powder again, reduce the deposition of powder at the seam crossing of ball grinder and ball milling cover to the disadvantageous effect of powder homogeneity, and in mechanical milling process, not taking off lid dandle again, is rock evenly by the deposition material powder being attached to ball grinder top equally; Sieve reunion grit for the second time that again remove and cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further.Repetition ball milling like this sieves and effectively can improve YAG transparent ceramic powder homogeneity.Employ the mode of twice ball milling in the preparation process in accordance with the present invention, and the rotating speed of the rotating ratio first time ball milling of second time ball milling is little, the mainly removing macrobead because second time has been sieved, remaining is all less particle, therefore the rotation speed requirements for second time ball milling is lower, only needs to select relatively little rotating speed to carry out ball milling and just can get a desired effect.Sieve order number is larger, and the particle sieved is less, and due under the effect of ball milling, the powder obtained will be more and more thinner, and therefore, sieve after second time ball milling the screen cloth needing to select order number larger, to remove the larger particle be difficult to ball milling method fragmentation further.
[beneficial effect]
In sum, compared to general YAG transparent ceramic powder ball-milling preparation method, it only includes once conventional mechanical milling process, and its beneficial features of meticulous, workable height provided by the invention even YAG transparent ceramic powder ball-milling preparation method is:
(1) add midway and take off the committed step of ball grinder dandle, its beneficial effect is can shake up the material powder that is deposited on ball grinder top and make it can be mixed by abundant ball milling in follow-up mechanical milling process;
(2) add the committed step of sieving, its beneficial effect is effectively to remove in slurry that those are difficult to by the reunion grit of ball mill crushing;
(3) committed step of slurry being carried out to secondary ball milling is added, its beneficial effect is again fully broken and blend feedstock powder, reduction powder in the seam crossing of ball grinder and ball milling cover and the deposition at ball grinder top to the disadvantageous effect of powder homogeneity.
Accompanying drawing explanation
Fig. 1 is that YAG ceramic powder SEM prepared by the embodiment of the present invention 1 schemes.
Embodiment
Fine method step in mechanical milling process is the emphasis exploratory development content of YAG crystalline ceramics technology of preparing, plays an important role to the YAG crystalline ceramics quality of final preparation.The mechanical milling process of YAG crystalline ceramics needs to reach simultaneously pulverizes feed particles and the even object of batch mixing.
Be described further below in conjunction with the ball-milling preparation method of specific embodiment to the even YAG transparent ceramic powder of height provided by the invention:
Embodiment 1:
Step (1): according to the YAG crystalline ceramics formula of design, by Al
2o
3, Y
2o
3, tetraethoxy and nano-MgO put into the ball grinder that aluminum oxide abrading-ball is housed successively after weighing, and then pours alcohol into; Wherein, Al
2o
3, Y
2o
3, the total mass of tetraethoxy and nano-MgO, aluminum oxide mill ball quality and alcohol mass ratio be: 1:5.7:1.6;
Step (2): will be fixed on planetary ball mill through step (1) charged ball grinder with the rotating speed ball milling 6 hours of 250r/min; Then taken off by ball grinder, do not take off lid dandle 10 times, object is the deposition material powder being attached to ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder rocked is fixed on planetary ball mill again, continues ball milling 6 hours according to the revolution of milling parameters 250r/min;
Step (3): the slurry after step (2) ball milling is poured in 400 object nylon mesh and sieves, object is to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further;
Step (4): in order to reduce the deposition of powder at the seam crossing of ball grinder and ball milling cover to the disadvantageous effect of powder homogeneity, the slurry obtained sieving through step (3) pour into again clean fill in the ball grinder of aluminum oxide abrading-ball, continue ball milling 6 hours according to the revolution of milling parameters 220r/min; Then taken off by ball grinder, do not take off and cover again dandle 10 times, object is to be continued by the material powder being deposited on ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder shaken is fixed on planetary ball mill again, continues ball milling 6 hours according to the revolution of milling parameters 220r/min;
Step (5): poured in 600 object nylon mesh by the slurry after step (4) ball milling and sieve, object is again to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further; The slurry this time obtained is the slurry after final ball milling, is passed through oven dry, sieve the even YAG transparent ceramic powder of height namely prepared as shown in Figure 1.
Described height even YAG transparent ceramic powder can obtain high-quality YAG crystalline ceramics through compressing tablet, sintering, polishing.
Embodiment 2:
Step (1): according to the YAG crystalline ceramics formula of design, by Al
2o
3, Y
2o
3, tetraethoxy and nano-MgO put into the ball grinder that aluminum oxide abrading-ball is housed successively after weighing, and then pours alcohol into; Wherein, Al
2o
3, Y
2o
3, the total mass of tetraethoxy and nano-MgO, aluminum oxide mill ball quality and alcohol mass ratio be: 1:5.7:1.7;
Step (2): will be fixed on planetary ball mill through step (1) charged ball grinder with the rotating speed ball milling 5 hours of 230r/min; Then taken off by ball grinder, do not take off lid dandle 7 times, object is the deposition material powder being attached to ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder rocked is fixed on planetary ball mill again, continues ball milling 5 hours according to the revolution of milling parameters 230r/min;
Step (3): the slurry after step (2) ball milling is poured in 300 object nylon mesh and sieves, object is to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further;
Step (4): in order to reduce the deposition of powder at the seam crossing of ball grinder and ball milling cover to the disadvantageous effect of powder homogeneity, the slurry obtained sieving through step (3) pour into again clean fill in the ball grinder of aluminum oxide abrading-ball, continue ball milling 5 hours according to the revolution of milling parameters 200r/min; Then taken off by ball grinder, do not take off and cover again dandle 7, object is to be continued by the material powder being deposited on ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder shaken is fixed on planetary ball mill again, continues ball milling 5 hours according to the revolution of milling parameters 200r/min;
Step (5): poured in 500 object nylon mesh by the slurry after step (4) ball milling and sieve, object is again to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further; The slurry this time obtained is the slurry after final ball milling, is passed through oven dry, namely sieve prepares the even YAG transparent ceramic powder of described height.
Described height even YAG transparent ceramic powder can obtain high-quality YAG crystalline ceramics through compressing tablet, sintering, polishing.
Embodiment 3:
Step (1): according to the YAG crystalline ceramics formula of design, by Al
2o
3, Y
2o
3, tetraethoxy and nano-MgO put into the ball grinder that aluminum oxide abrading-ball is housed successively after weighing, and then pours alcohol into; Wherein, Al
2o
3, Y
2o
3, the total mass of tetraethoxy and nano-MgO, aluminum oxide mill ball quality and alcohol mass ratio be: 1:5.7:1.8;
Step (2): will be fixed on planetary ball mill through step (1) charged ball grinder with the rotating speed ball milling 3 hours of 220r/min; Then taken off by ball grinder, do not take off lid dandle 5 times, object is the deposition material powder being attached to ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder rocked is fixed on planetary ball mill again, continues ball milling 3 hours according to the revolution of milling parameters 220r/min;
Step (3): the slurry after step (2) ball milling is poured in 200 object nylon mesh and sieves, object is to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further;
Step (4): in order to reduce the deposition of powder at the seam crossing of ball grinder and ball milling cover to the disadvantageous effect of powder homogeneity, the slurry obtained sieving through step (3) pour into again clean fill in the ball grinder of aluminum oxide abrading-ball, continue ball milling 3 hours according to the revolution of milling parameters 160r/min; Then taken off by ball grinder, do not take off and cover again dandle 5, object is to be continued by the material powder being deposited on ball grinder top to rock evenly, then by abundant ball milling; Then the ball grinder shaken is fixed on planetary ball mill again, continues ball milling 3 hours according to the revolution of milling parameters 160r/min;
Step (5): poured in 400 object nylon mesh by the slurry after step (4) ball milling and sieve, object is again to remove the reunion grit that cannot rely on ball mill crushing in raw material, improves the homogeneity of ball milling material powder further; The slurry this time obtained is the slurry after final ball milling, is passed through oven dry, namely sieve prepares the even YAG transparent ceramic powder of described height.
Described height even YAG transparent ceramic powder can obtain high-quality YAG crystalline ceramics through compressing tablet, sintering, polishing.
In order to verify the beneficial effect of the ball-milling preparation method adopting the even YAG transparent ceramic powder of meticulous, workable height provided by the invention, we also adopt general YAG crystalline ceramics ball milling method to be two groups of contrast experiments:
Contrast experiment 1:
Step is: according to the YAG crystalline ceramics formula of design, by Al
2o
3, Y
2o
3, tetraethoxy and nano-MgO put into the ball grinder that aluminum oxide abrading-ball is housed after weighing, then alcohol is poured into, with the rotating speed ball milling 24 hours of 220r/min on planetary ball mill, wherein, the mass ratio of YAG material powder, aluminum oxide abrading-ball and dehydrated alcohol is: 1:5.7:1.6; The slurry obtained is the slurry after final ball milling, is passed through oven dry, sieves, compressing tablet, sintering, polishing can obtain high uniformity YAG crystalline ceramics.
Contrast experiment 2:
Step is: according to the YAG crystalline ceramics formula of design, by Al
2o
3, Y
2o
3, tetraethoxy and nano-MgO put into the ball grinder that aluminum oxide abrading-ball is housed after weighing, then alcohol is poured into, on planetary ball mill with the rotating speed ball milling 16 hours of 180r/min wherein, the mass ratio of YAG material powder, aluminum oxide abrading-ball and dehydrated alcohol is: 1:5.7:1.8; The slurry obtained is the slurry after final ball milling, is passed through oven dry, sieves, compressing tablet, sintering, polishing can obtain high uniformity YAG crystalline ceramics.
Slurry after the final ball milling obtain embodiment 1 ~ 3 and contrast experiment 1 ~ 2 crosses 700 nylon mesh respectively, then by nylon mesh rinsing 2 minutes in water, to remain in nylon mesh Raw reunion grit is collected in glass culture dish, the quality of residual reunion grit is weighed after drying, then the mass percent of residual reunion grit in material powder calculated is as shown in table 1, therefrom can find out that the ball-milling preparation method of the even YAG transparent ceramic powder of height provided by the invention effectively can remove the reunion grit that cannot rely on ball mill crushing in raw material, improve the homogeneity of raw material ball abrasive dust body.
Table 1 remains the mass percent of reunion grit in material powder (%)
Slurry after the final ball milling that embodiment 1 ~ 3 and contrast experiment 1 ~ 2 are obtained, passed through oven dry, sieved, YAG crystalline ceramics as shown in table 2 in the transmitance at 1064nm wavelength place that compressing tablet, sintering, polishing obtain, showing that the ball-milling preparation method of the even YAG transparent ceramic powder of height provided by the invention effectively can improve the homogeneity of raw material ball abrasive dust body, having established solid powder basis for preparing high-quality YAG pottery.
The transmitance (%) of table 2YAG crystalline ceramics at 1064nm wavelength place
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Contrast experiment 1 | Contrast experiment 2 | |
| Transmitance (%) | 83.3 | 83.1 | 82.7 | 80.8 | 77.1 |
In sum, the invention provides a kind of ball-milling preparation method of meticulous, the workable even YAG transparent ceramic powder of height, the method can fully broken and blend feedstock powder, and reduces powder in the seam crossing of ball grinder and ball milling cover and the deposition at ball grinder top to the disadvantageous effect of powder homogeneity.And the YAG transparent ceramic powder utilizing preparation method of the present invention to prepare is prepared into YAG crystalline ceramics further, its transmitance at 1064nm wavelength place all >=82%.
Claims (4)
1. a high even YAG transparent ceramic powder ball-milling preparation method, it is characterized in that comprising ball milling, rock, sieve and slurry secondary ball milling four Key detail processes, its concrete steps are as follows:
Step (1): according to the YAG crystalline ceramics formula of design, by Al
2o
3, Y
2o
3, tetraethoxy and nano-MgO put into the ball grinder that aluminum oxide abrading-ball is housed successively after weighing, and then pours alcohol into;
Step (2): will be fixed on planetary ball mill through step (1) charged ball grinder with the rotating speed ball milling 3 ~ 6 hours of 220 ~ 250r/min; Then ball grinder is taken off, do not take off lid dandle 5 ~ 10 times; Then ball grinder is fixed on planetary ball mill again, continues ball milling 3 ~ 6 hours according to parameter 220 ~ 250r/min;
Step (3): the slurry after step (2) ball milling is poured in 200 ~ 400 object nylon mesh and sieves;
Step (4): the slurry obtained sieving through step (3) pour into again clean fill in the ball grinder of aluminum oxide abrading-ball, continue ball milling 3 ~ 6 hours according to the rotating speed of milling parameters 160 ~ 220r/min; Then ball grinder is taken off, do not take off and cover again dandle 5 ~ 10 times; Then ball grinder is fixed on planetary ball mill again, continues ball milling 3 ~ 6 hours according to parameter 160 ~ 220r/min;
Step (5): the slurry after step (4) ball milling is poured in 400 ~ 600 object nylon mesh and sieves; The slurry this time obtained is the slurry after final ball milling, is passed through oven dry, namely sieve prepares the even YAG transparent ceramic powder of described height.
2. height according to claim 1 even YAG transparent ceramic powder ball-milling preparation method, is characterized in that in described step (1), Al
2o
3, Y
2o
3, the total mass of tetraethoxy and nano-MgO, aluminum oxide mill ball quality and alcohol mass ratio be 1:5.7:1.6 ~ 1.8.
3. height according to claim 1 even YAG transparent ceramic powder ball-milling preparation method, is characterized in that the rotational speed of ball-mill of described step (2) is greater than the rotational speed of ball-mill of described step (4).
4. height according to claim 1 even YAG transparent ceramic powder ball-milling preparation method, is characterized in that the nylon grit number of described step (3) is less than the nylon grit number of described step (5).
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| CN105523753A (en) * | 2016-01-06 | 2016-04-27 | 中国科学院上海光学精密机械研究所 | Visible/shortwave infrared/mediumwave infrared YAG transparent ceramic and preparation method thereof |
| CN110526295A (en) * | 2019-07-16 | 2019-12-03 | 东北大学 | One kind mixing ytterbium Gadolinium Tungstate potassium nano crystal particles and preparation method thereof |
| CN111302296A (en) * | 2019-11-19 | 2020-06-19 | 中国工程物理研究院电子工程研究所 | Method for micro-nano electroforming micro device |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105523753A (en) * | 2016-01-06 | 2016-04-27 | 中国科学院上海光学精密机械研究所 | Visible/shortwave infrared/mediumwave infrared YAG transparent ceramic and preparation method thereof |
| CN105523753B (en) * | 2016-01-06 | 2018-05-08 | 中国科学院上海光学精密机械研究所 | It can be seen that/short-wave infrared/medium-wave infrared YAG crystalline ceramics and its manufacture method |
| CN110526295A (en) * | 2019-07-16 | 2019-12-03 | 东北大学 | One kind mixing ytterbium Gadolinium Tungstate potassium nano crystal particles and preparation method thereof |
| CN110526295B (en) * | 2019-07-16 | 2021-05-14 | 东北大学 | Ytterbium-doped potassium gadolinium tungstate nanocrystal particle and preparation method thereof |
| CN111302296A (en) * | 2019-11-19 | 2020-06-19 | 中国工程物理研究院电子工程研究所 | Method for micro-nano electroforming micro device |
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Application publication date: 20151202 |