CN107661741B - Method for preparing mesoporous selective adsorption material to treat hexamethyldisilazane - Google Patents
Method for preparing mesoporous selective adsorption material to treat hexamethyldisilazane Download PDFInfo
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Abstract
The invention discloses a method for preparing a mesoporous selective adsorption material to treat hexamethyldisilazane, which comprises the following steps: s1, preparing a mesoporous selective adsorption material; s2, placing the mesoporous selective adsorption material in an adsorption reactor; s3, conveying the waste gas containing hexamethyldisilazane to an adsorption reactor for adsorption to remove the hexamethyldisilazane; the adsorption reactor consists of a shell, a plurality of stand columns, a plurality of adsorption plates and a temperature control device; the adsorption plate is internally filled with a mesopore selective adsorption material, and uniformly distributed air holes are formed in the upper surface and the lower surface; the inside a plurality of stands that set up of casing, the adsorption plate is fixed between adjacent stand, and all adsorption plates and stand splice each other and form a cockscomb structure or comb-tooth's whole adsorption wall. The invention adopts the adsorbing material with selective adsorbability and the corresponding adsorption reactor to adsorb and remove hexamethyldisilazane in the waste gas, simplifies the subsequent treatment process of the waste gas, and obviously reduces the energy consumption and the economic cost.
Description
Technical Field
The invention relates to a method for preparing a mesoporous selective adsorption material for adsorbing and removing hexamethyldisilazane contained in waste gas, belonging to the technical field of waste gas treatment.
Background
Bis (trimethylsilyl) amine (also known as hexamethyldisilazane, or HMDS) of the formula [ (CH)3)3Si]2And (4) NH. The substance is a derivative in which two hydrogen atoms in ammonia are substituted by trimethylsilyl groups. Hexamethyldisilazane is a colorless liquid and is also an important reagent and main component widely used in organic synthesis and organometallic chemical reactions. In photolithography, hexamethyldisilazane is often used as an adhesion promoter to increase the adhesion of the photoresist surface. Hexamethyldisilazane in the gaseous state gives the best results on the heated substrate. Hexamethyldisilazane can be used as a drying agent for critical point drying during sample preparation under electron microscopy. In cleavage gas liquid chromatography, hexamethyldisilazane is added to the analyte upon cleavage to produce a silylated analyte and to enhance the detectability of the compound with polar functional groups.
HMDS is one of the Volatile Organic Compounds (VOCs), which refers to Organic Compounds having a vapor pressure greater than 0.1mmHg under standard conditions (20 ℃, 760 mmHg). HMDS is mainly derived from the fields of optoelectronic materials and device manufacturing, semiconductor industry, and the like. The current methods for treating HMDS include condensation, thermal incineration, catalytic incineration, plasma destruction, and adsorption. Among them, the condensation method has a limited treatment efficiency. Catalytic incineration and thermal incineration require high temperatures to destroy the VOCs, require large amounts of fuel, and create particle problems that increase the cost of secondary processing. The plasma damage method will disturb the machine, the maintenance cost is high, the manufacturing cost of the power supply is expensive, and the manufacturing technology still has a bottleneck. The adsorption method has high treatment efficiency, short time, low requirement on temperature, small occupied area of equipment, low fuel consumption, large treatment capacity and no trouble of generating secondary pollutants due to high temperature, can be carried out in a low-temperature environment, and is the most promising technology for treating the HMDS at present.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
It is still another object of the present invention to organically combine the adsorption method with the incineration method to solve the technical problems of high incineration temperature, high energy consumption, large amount of fuel requirement, particle generation, blockage of the incineration vessel, increase of secondary treatment cost, etc. in the prior art of incineration method for treating waste gas containing silane.
To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, there is provided a method for preparing a mesoporous selective adsorbent material for treating hexamethyldisilazane, comprising the steps of:
s1, preparing a mesoporous selective adsorption material;
s2, placing the prepared mesoporous selective adsorption material in an adsorption reactor;
s3, controlling the temperature in the adsorption reactor to be 25-70 ℃, and then conveying the waste gas containing hexamethyldisilazane to be treated into the adsorption reactor for selective adsorption to remove hexamethyldisilazane;
the adsorption reactor consists of a box-shaped shell, a plurality of stand columns, a plurality of square adsorption plates and a temperature control device; the adsorption plate is internally filled with prepared selective adsorption material with mesopores, and the upper surface and the lower surface of the adsorption plate are provided with uniformly distributed air holes;
the two opposite side surfaces of the shell are respectively provided with an air inlet and an air outlet, and the top surface of the shell is of a detachable structure; a plurality of upright columns which are uniformly distributed are vertically arranged in the shell from the top surface to the bottom surface of the shell, two strip-shaped limiting grooves for installing adsorption plates are arranged on the surfaces of the upright columns along the axis direction, the adsorption plates are fixed between the adjacent upright columns in an insertion manner along the limiting grooves of the upright columns, and all the adsorption plates and the upright columns are spliced with each other to form a zigzag or comb-shaped integral adsorption wall; the adsorption wall divides the shell into two parts, one part comprises an air inlet and an untreated waste gas circulation space communicated with the air inlet, and the other part comprises an air outlet and a treated waste gas circulation space; the joints of the adjacent adsorption plates and the joints of the adsorption plates and the inner wall surface of the shell are completely sealed in a mode that gas cannot pass through;
the temperature control device comprises a heating element and a temperature sensor which are positioned in the shell, and a controller which is positioned outside the shell and is connected with the heating element and the temperature sensor.
Preferably, the step S1 specifically includes:
s11, dissolving cetyl trimethyl ammonium bromide in deionized water, and adding an ammonium hydroxide solution with the mass concentration of 28% to obtain an organic solution;
s12, dropwise adding the silicon source solution into the organic solution, adjusting the pH value of the solution to 4 by using sulfuric acid, and stirring and reacting for 8 hours at room temperature;
s13, filtering, washing and drying the mixed solution obtained in the step S12 to obtain a primary finished product;
and S14, carrying out high-temperature calcination on the primary product, removing the organic template, and preparing the granular mesoporous selective adsorption material.
Further preferably, the molar ratio of each raw material component in the step S1 is: cetyl trimethylammonium bromide: NH4 OH: si 145: 3.5: 1.5.
preferably, in step S13, the filtered filter cake is washed with deionized water and alcohol, and then dried in an oven at 100 ± 5 ℃ for 4-8 h.
Preferably, in the step S14, the primary product is calcined at 550 ℃ for 6 hours to obtain the granular mesoporous selective absorbing material.
Preferably, the concentration of hexamethyldisilazane in the exhaust gas containing hexamethyldisilazane is 500 to 2000 ppm.
Preferably, the flow rate of the waste gas to be treated entering the adsorption reactor is 100-800 mL/min, and the retention time of the waste gas in the adsorption reactor is 0.4-2.4 seconds.
Preferably, the heating element is disposed within the housing adjacent to the inlet port, and the temperature sensor is disposed within the housing in an untreated exhaust gas flow space communicating with the inlet port.
Preferably, barometers are respectively disposed in the two divided portions of the housing.
Preferably, the upper and lower surfaces of the adsorption plate are provided with metal mesh layers, the edges of the adsorption plate are wrapped and sealed by strip-shaped metal sheets, the space between the two metal mesh layers is filled with mesoporous hole selective adsorption material particles, the particle size of the adsorption material is larger than the aperture of the metal mesh, the side edge of the adsorption plate, which is in contact with the upright post, is provided with a convex part, and the convex part is embedded into a limit groove of the upright post and fixedly connected with the limit groove through a screw.
Compared with the prior art, the invention has the advantages that:
firstly, the prepared mesoporous selective adsorption material has the performance of selectively adsorbing the silane (HMDS) in the waste gas, even if the mesoporous selective adsorption material is operated for a long time, the adsorption performance of the adsorption material is still good, the treatment efficiency can still reach more than 99 percent after the mesoporous selective adsorption material is continuously used for 140min, the penetration point is not reached, and the good adsorption effect can still be maintained.
And secondly, the HMDS in the waste gas is removed through adsorption treatment, so that the subsequent treatment process steps are simplified, and the subsequent treatment cost is effectively reduced.
And thirdly, the self-made granular mesoporous selective adsorption material is adopted, the preparation method is simple, the granular adsorption material is pre-processed into an adsorption plate unit, and the adsorption plate is assembled in a specific adsorption reactor to form a novel adsorption reactor for treating the waste gas containing HDMS under the low-temperature condition, so that the adsorption reaction condition is mild, and the adsorption effect is good.
Fourthly, make the adsorption plate with granule adsorbing material in advance, left out the operation that the job site directly loaded the adsorption particle to the adsorption reactor, avoided the scene to load the granule that exists and load unevenly, and the extravagant scheduling problem that scatters easily, the adsorption effect that adopts the adsorption plate is better, and its installation, dismantlement, operation such as change adsorbing material are more simple and convenient.
Drawings
FIG. 1 is a schematic view of the structure of an adsorption reactor.
Fig. 2, top view of an adsorption reactor.
Fig. 3 is a top view of an adsorption reactor in another embodiment.
Fig. 4, a top view and a longitudinal section of the pillar in the embodiment.
Fig. 5 is a schematic structural view of the adsorption plate in the embodiment.
FIG. 6 is a scanning electron microscope image of the mesoporous selective adsorbent.
FIG. 7 shows a reaction diagram of HDMS adsorption using mesoporous selective adsorption material.
FIG. 8 is a graph showing the results of adsorption treatment of exhaust gas generated in a semiconductor factory by the method of the present invention.
FIG. 9 is a graph showing the results of continuously testing the adsorption treatment of the exhaust gas generated from a semiconductor manufacturing plant according to the method of the present invention.
FIG. 10 is an Arrhenius model diagram of the porous selective adsorbent of the present invention.
FIG. 11 shows the comparison between the measured values of the experiment of the present invention and the pattern prediction results.
Reference numbers in the figures:
the device comprises a shell 1, an air inlet 11, an air outlet 12, a stand column 2, a limiting groove 21, an adsorption plate 3, a metal mesh layer 31, a metal sheet 32, adsorbent particles 33, a convex part 34, a temperature control device 4, a heating element 41, a temperature sensor 42, a controller 43 and a barometer 5.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
The preparation method of the hole selective adsorption material comprises the following steps:
s11, preparing an organic solution: 2.5g of cetyltrimethylammonium bromide (CTABr) is weighed and dissolved in 125 ml of deionized water, 10 ml of ammonium hydroxide solution with the mass concentration of 28 wt% is added, and stirring is continuously carried out for 15 minutes at room temperature through a magnetic stirrer, so that the cetyltrimethylammonium bromide (CTABr) is completely dissolved.
S12, preparing a mixed solution: the silicon source solution was added dropwise to the organic solution prepared in step S11, and the pH was adjusted to 4 with 4mol/L sulfuric acid solution, and the mixture was continuously stirred for 8 hours at room temperature through a magnetic stirrer.
S13, preparing a primary finished product, filtering the mixed solution in the step S12, washing with deionized water and alcohol, and drying in an oven at 100 +/-5 ℃ for 4 to 8 hours.
And S14, placing the dried primary product into a high-temperature furnace, calcining for 6 hours at the temperature of 550 ℃, removing the organic template, and preparing the granular mesoporous selective adsorption material.
The molar ratio of each raw material component in the preparation process is as follows: cetyl trimethylammonium bromide: NH4 OH: si 145: 3.5: 1.5.
and placing the prepared mesoporous selective adsorption material in an adsorption reactor. As shown in fig. 1 to 4, the adsorption reactor is composed of a box-shaped casing 1, a plurality of columns 2, a plurality of square adsorption plates 3, and a temperature control device 4. The side of the shell is made of transparent material. The upright is made of metal. The adsorption plate 3 is filled with prepared mesoporous hole selective adsorption material 33, and the upper surface and the lower surface of the adsorption plate are provided with uniformly distributed air holes. The relative both sides face of casing 1 sets up air inlet 11 and gas outlet 12 respectively, and the top surface of casing 1 is detachable structure, the installation of the adsorption plate 3 of being convenient for. Inside from the casing top surface to the bottom surface of casing 1 upright sets up a plurality of stands 2 of evenly distributed, 2 surfaces of stand set up two bar spacing grooves 21 that are used for installing the adsorption plate along the axis direction, and adsorption plate 3 inserts along the spacing groove 21 of stand and fixes between adjacent stand 2, and all adsorption plates 3 and stand 2 splice each other and form a cockscomb structure or comb-tooth's whole adsorption wall (see fig. 2 and fig. 3 respectively). The adsorption wall divides the shell into two parts, one part comprises an air inlet 11 and an untreated waste gas circulation space a communicated with the air inlet, and the other part comprises an air outlet 12 and a treated waste gas circulation space b; the joint between adjacent adsorption plates 3 and the joint between the adsorption plate 3 and the inner wall surface of the casing 1 are completely sealed in such a manner that gas cannot pass through them. Barometers 5 are respectively arranged in the two split parts of the shell, and further preferably, a single chip microcomputer, an alarm and a display screen are arranged outside the shell, and the single chip microcomputer is respectively connected with the two barometers, the alarm and the display screen. The working principle is as follows: the atmospheric pressure value that the barometer surveyed is transmitted for the singlechip, and the display screen is transmitted with the atmospheric pressure value to the singlechip, and the staff can look over the atmospheric pressure value through the display screen. When the air pressure value is higher than a certain set value, the single chip microcomputer controls the alarm to give an alarm to remind workers that the air pressure in the reactor is higher, and relevant remedial measures are taken in time to reduce the air pressure.
The temperature control device 4 comprises a heating element 41 and a temperature sensor 42 which are positioned in the shell 1, and a controller 43 which is positioned outside the shell 1 and is connected with the heating element 41 and the temperature sensor 42. Specifically, the method comprises the following steps: a heating element 41 is provided in the housing near the intake port 11, and a temperature sensor 42 is provided in the housing in the untreated exhaust gas flow-through space a communicating with the intake port. Another embodiment is also possible: the heating elements 41 are resistance wires which are uniformly distributed on the bottom and side surfaces inside the housing 1, and are further limited to be disposed on the bottom and side surfaces inside the housing which are occupied by the air inlet 11 and the untreated exhaust gas flowing space a communicating with the air inlet.
In another embodiment, as shown in fig. 5, the specific structure of the adsorption plate 3 is as follows: the upper and lower surfaces of the adsorption plate 3 are provided with metal mesh layers 31, the edges of the adsorption plate are wrapped and sealed by strip-shaped metal sheets 32, the space between the two metal mesh layers 31 is filled with middle-hole selective adsorption material particles 33, and the particle size of the adsorption material is larger than the aperture of the metal mesh. The side edge of the adsorption plate 3 contacting with the upright column 2 is provided with a convex part 34, and the convex part 34 is embedded into the limit groove 21 of the upright column and fixedly connected with the limit groove through a screw.
And after the adsorption reactor is installed, adjusting and controlling the temperature in the adsorption reactor to be 25-70 ℃, and then conveying the waste gas containing hexamethyldisilazane to be treated into the adsorption reactor for selective adsorption to remove hexamethyldisilazane. Waste gas enters the adsorption reaction container from the gas inlet, flows in the untreated waste gas circulation space a, and contacts with the adsorption plate 3, because the connection part of the adsorption plate 3 and the inner wall surface of the shell is completely closed in a way that the waste gas can not pass through, the waste gas can only pass through gaps among the adsorbent particles in the adsorption plate 3, and in the process, the waste gas is fully contacted with the adsorbent material, HDMS in the waste gas is selectively adsorbed, and the waste gas after adsorption treatment is discharged from the gas outlet, so that the purpose of waste gas adsorption treatment is achieved. Wherein the concentration of hexamethyldisilazane in the exhaust gas containing hexamethyldisilazane is 500-2000 ppm. The flow rate of the waste gas to be treated entering the adsorption reactor is 100-800 mL/min, and the retention time of the waste gas in the adsorption reactor is 0.4-2.4 seconds.
Performance analysis and application examples:
scanning electron microscope analysis, nitrogen isothermal adsorption/desorption instrument characteristic analysis and adsorption performance analysis were performed on the mesoporous selective adsorption material prepared in the above examples, and the adsorption behavior of the mesoporous selective adsorption material for treating HDMS in the present invention was investigated using freund delrich model (Freundlich model), Langmuir model (Langmuir model) and Arrhenius model (Arrhenius model).
A, B in FIG. 6 is an SEM image of the mesoporous and mesoporous selective adsorbent material of the invention. In SEM, it is obvious that the shape of the mesoporous selective adsorbing material is spherical, and the mesoporous selective adsorbing material is synthesized by the surfactant and the silicate together and has the particle shapes of round, oval and the like.
And (4) analyzing the characteristics of the nitrogen isothermal adsorption/desorption instrument of the mesoporous adsorption material. Table 1 shows the results of the specific surface area and pore size tests of the adsorbent materials. It can be seen that the specific surface area of the mesoporous selective adsorbent material is 908.5 + -18 m2Per g, with an average pore volume of 0.598cm3In g, the pore size distribution is centered at 2.62 nm.
TABLE 1 specific surface area and pore size of the adsorbent materials
In order to investigate the adsorption capacity of the mesoporous selective adsorbent material for HMDS, an adsorption experiment was performed by feeding an exhaust gas containing HMDS at a concentration of 100ppm and 500ppm to an adsorption reactor at a flow rate of 100mL/min (residence time of 2.8 seconds), respectively, and the experimental results are shown in fig. 7. It can be seen that the breakthrough times were 1070min and 340min, respectively, and the adsorption amounts were 40mg/g and 86mg/g, respectively.
The treatment method of the invention is adopted to adsorb and treat the waste gas generated by a certain semiconductor factory (the treatment flow is 10 m)3Min), the results are shown in FIGS. 8 and 9. It can be seen that the treatment efficiency can reach more than 97% through continuous test results of 3 days, which proves that the adsorbing material can efficiently treat the waste gas generated by a semiconductor factory.
The results of the Vermilion model (Freundlich model) and Langmuir model (Langmuir model) analyses of the pore-selective adsorbent material of the present invention are shown in Table 2. FIG. 10 is an Arrhenius model (Arrhenius model) of the porous selective adsorbent material of the present invention. As shown in Table 3, it can be seen from the Arrhenius equation that the rate of change of lnk (k is a reaction rate constant) with T is proportional to the activation energy Ea. Thus, the higher the activation energy, the faster the reaction rate increases with increasing temperature, and the more sensitive the reaction rate is to temperature. If a plurality of reactions having different activation energy values coexist, a high temperature is advantageous for a reaction having a high activation energy, and a low temperature is advantageous for a reaction having a low activation energy.
TABLE 2 isothermal adsorption mode
TABLE 3 Arrhenius model parameter calculation
As shown in fig. 11, the calculated value of Freundlich is very close to the actual value. Therefore, in the single-component adsorption system of the present experiment, it is suitable to describe the adsorption behavior of the pore-selective adsorption material in the Freundlich model.
In conclusion, the method for treating HMDS by using the prepared mesoporous selective adsorption material has high adsorption treatment efficiency, and even if the adsorption material is operated for a long time, the adsorption performance of the adsorption material is still good, the penetration point is not reached, and the good adsorption effect can be still maintained.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A method for preparing a mesoporous selective adsorption material for treating hexamethyldisilazane, comprising the following steps:
s1, preparing a mesoporous selective adsorption material; the method comprises the following specific steps:
s11, dissolving cetyl trimethyl ammonium bromide in deionized water, and adding an ammonium hydroxide solution with the mass concentration of 28% to obtain an organic solution;
s12, dropwise adding the silicon source solution into the organic solution, adjusting the pH value of the solution to 4 by using sulfuric acid, and stirring and reacting for 8 hours at room temperature;
s13, filtering, washing and drying the mixed solution obtained in the step S12 to obtain a primary finished product;
s14, high-temperature calcination is carried out on the primary finished product, the organic template is removed, and the granular mesoporous selective adsorption material is prepared;
s2, placing the prepared mesoporous selective adsorption material in an adsorption reactor;
s3, controlling the temperature in the adsorption reactor to be 25-70 ℃, and then conveying the waste gas containing hexamethyldisilazane to be treated into the adsorption reactor for selective adsorption to remove hexamethyldisilazane;
the adsorption reactor consists of a box-shaped shell, a plurality of stand columns, a plurality of square adsorption plates and a temperature control device; the adsorption plate is internally filled with prepared selective adsorption material with mesopores, and the upper surface and the lower surface of the adsorption plate are provided with uniformly distributed air holes; the two opposite side surfaces of the shell are respectively provided with an air inlet and an air outlet, and the top surface of the shell is of a detachable structure; a plurality of upright columns which are uniformly distributed are vertically arranged in the shell from the top surface to the bottom surface of the shell, two strip-shaped limiting grooves for installing adsorption plates are arranged on the surfaces of the upright columns along the axis direction, the adsorption plates are fixed between the adjacent upright columns in an insertion manner along the limiting grooves of the upright columns, and all the adsorption plates and the upright columns are spliced with each other to form a zigzag or comb-shaped integral adsorption wall; the adsorption wall divides the inner space of the shell into two parts, one part comprises an air inlet and an untreated waste gas circulation space communicated with the air inlet, and the other part comprises an air outlet and a treated waste gas circulation space; the joints of the adjacent adsorption plates and the joints of the adsorption plates and the inner wall surface of the shell are completely sealed in a mode that gas cannot pass through;
the temperature control device comprises a heating element and a temperature sensor which are positioned in the shell, and a controller which is positioned outside the shell and is connected with the heating element and the temperature sensor.
2. The method for preparing a mesoporous selective adsorbent material for treating hexamethyldisilazane according to claim 1, wherein the molar ratio of each raw material component in step S1 is: cetyl trimethylammonium bromide: NH (NH)4OH：Si＝145：3.5：1.5。
3. The method for preparing a mesoporous selective absorbing material to treat hexamethyldisilazane according to claim 2, wherein in step S13, the filtered filter cake is washed with deionized water and alcohol, and then dried in an oven at 100 ± 5 ℃ for 4-8 h.
4. The method for preparing a mesoporous selective adsorbent material to treat hexamethyldisilazane according to claim 3, wherein in step S14, the primary product is calcined at 550 ℃ for 6h to obtain a granular mesoporous selective adsorbent material.
5. The method for preparing a mesoporous selective adsorbent material to treat hexamethyldisilazane according to claim 4, wherein the concentration of hexamethyldisilazane in the exhaust gas containing hexamethyldisilazane is 500-2000 ppm.
6. The method for preparing a mesoporous selective absorbing material for treating hexamethyldisilazane according to claim 5, wherein the flow rate of the waste gas to be treated entering the adsorption reactor is 100-800 mL/min, and the residence time of the waste gas in the adsorption reactor is 0.4-2.4 seconds.
7. The method of claim 1, wherein the heating element is disposed within the housing proximate the inlet port, and the temperature sensor is disposed within an untreated exhaust gas plenum in the housing in communication with the inlet port.
8. The method according to claim 7, wherein barometers are respectively disposed in the two divided portions of the housing.
9. The method for preparing mesoporous selective absorbing material to treat hexamethyldisilazane according to claim 1, wherein metal mesh layers are disposed on the upper and lower surfaces of the absorbing plate, the edges of the absorbing plate are wrapped and sealed by strip-shaped metal sheets, the space between the two metal mesh layers is filled with mesoporous selective absorbing material particles, the particle size of the absorbing material is larger than the pore size of the metal mesh, a protrusion is disposed on the side edge of the absorbing plate contacting with the upright post, and the protrusion is embedded into the limiting groove of the upright post and fixedly connected with the limiting groove by a screw.
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| CN1948161A (en) * | 2006-10-19 | 2007-04-18 | 复旦大学 | Nano-crystal large poresize mesopore oxide material and its preparation method |
| CN205650034U (en) * | 2016-05-31 | 2016-10-19 | 淮阴师范学院 | Plate and frame gas adsorbing device |
| CN106353426A (en) * | 2016-08-31 | 2017-01-25 | 科邦检测集团有限公司 | Badge type passive air sampler based on MCM-41 molecular sieve |
| CN106943843A (en) * | 2017-03-24 | 2017-07-14 | 佛山市南海依泰科空气处理设备有限公司 | A kind of waste gas adsorption runner body and preparation method thereof and equipment |
Non-Patent Citations (1)
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| Treatment of Volatile Organic Compounds with Mesoporous Materials Prepared from Calcium Fluoride Sludge;Sy-Yuan Kang et al.;《J. Nanosci. Nanotechnol.》;20161231;第16卷(第2期);摘要，第1962页第2节，表1 * |
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| CN107661741A (en) | 2018-02-06 |
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