CN102389754A - Mesoporous macromolecule/silicon oxide nanocomposite with layered channel structure and preparation method thereof - Google Patents
Mesoporous macromolecule/silicon oxide nanocomposite with layered channel structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a mesoporous macromolecule/silicon oxide nanocomposite with a one-dimensional layered channel structure. The preparation method of the nanocomposite comprises the following steps: using PDMS-PEO and P123 as mixed structure directing agent, and phenolic resin prepolymer as carbon source precursor to mix, reacting to obtain an As-made intermediate, and then roasting to obtain the nanocomposite. In the small angle X-ray scattering (SAXS) map of the As-made intermediate has the diffraction peaks of which ratio of three q values is 1:2:3. The thermal stability range of the layered structure of the nanocomposite is 300-380 DEG C, the spacing of layers is 8-15nm and the specific surface area, pore volume and pore diameter are 500-900m<2>/g, 0.40-0.58cm<3>/g and 4.5-5.6nm respectively. The nanocomposite is particularly suitable for the fields such as low dielectric constant coatings, membrane separation, sensors and optical materials. Meanwhile, the expensive silane reagent is not required to be introduced in the preparation method and the traditional sol-gel process can be avoided, thus the preparation process of the mesoporous macromolecule/silicon oxide nanocomposite can be greatly simplified and a new synthetic route of the economical and reasonable mesoporous macromolecule/silicon oxide nanocomposite with high maneuverability is developed.
Description
Technical field
The invention belongs to the nanometer new material technology field; Relate in particular to meso-porous nano composite of a kind of tool one dimension stratiform pore passage structure and preparation method thereof, be specifically related to mesoporous polymer/monox nanometer composite of a kind of tool one dimension stratiform pore passage structure and preparation method thereof.
Background technology
Organic not only has the pliability, hydrophobic and be prone to functionalized characteristics of organic component, also has performances such as high heat endurance of inorganic component and mechanical strength simultaneously.For the meso-porous nano composite; Not only have duct size evenly, arrange in order, can be 2 ~ 50nm scope in the continuous excellent characteristic such as adjustable in aperture; But also have unique nanometer three-dimensional effect, thereby has important potential use in many fields such as catalysis, absorption, separation, opto-electronic device and electrode material for super capacitor.
Mesoporous polymer/monox nanometer composite is a kind of important meso-porous nano composite, has better heat, conduction, machinery and chemical property etc. than single mesoporous polymer or meso pore silicon oxide material.Simultaneously, the silica component in the system can effectively overcome shortcomings such as skeleton shrinks seriously in the simple organic system carbonisation, the aperture is little, specific area is low.
At present, the synthetic method of mesoporous polymer/monox nanometer composite mainly contains the functionalisation of surfaces of mesopore silicon oxide, back grafting and ternary assemble method altogether.The functionalisation of surfaces method of mesopore silicon oxide is to utilize to contain the silicon source of organic functional group or the special functionalized mesoporous organic silicon oxide of surfactant synthetic surface; Silica reagent and surfactant expensive raw materials and be difficult to synthesize in this method are unfavorable for producing in enormous quantities; Back grafting is filled polymer or a carbon in meso pore silicon oxide material, and this method complex operation, uneconomical, and the very difficult control of polymerization process cause the duct to stop up easily; Ternary construction from part altogether is that the advanced material laboratory Zhao Dongyuan of Fudan University professor seminar took the lead in reporting in 2006; At first assemble synthesising mesoporous macromolecule/monox nanometer composite altogether through the ternary of commercial triblock copolymer, ethyl orthosilicate and phenolic resins performed polymer; This method has overcome the shortcoming of preceding two kinds of methods, but adopts this method only can obtain having the mesoporous polymer/monox nanometer composite of two dimension six side p6m structures.And the mesoporous polymer/monox nanometer composite with one dimension stratiform pore passage structure is not seen bibliographical information so far.
Silicon-containing surfactant is a kind of novel surfactant that grows up along with the organosilicon new material; In water and non-aqueous system, all has excellent surface activity; Surface tension is reduced to about 20 mN/m; Also have good wetting and spreadability at low-energy surface, also have characteristics such as Heat stability is good, physiological safety simultaneously.Block copolymer dimethyl silicone polymer-polyoxyethylene (PDMS-PEO) is a kind of novel organosilicon surfactant, do as one likes can difference very big polysiloxanes segment be connected through chemical bond with polyether segment and form.Wherein, Polysiloxanes is siliceous organic compound, and the silicon structure that alternately occurs is given its many good performances, like low surface tension; Good viscosity temperature characteristic, compliance and in polar surfaces spread property and excellent hydrophobic property and the serviceability etc. that is adapted under the wide temperature range; Hydrophilic polyether segment is given polysiloxanes with water-soluble, makes excellent properties such as its high-low temperature resistant that had both had traditional polysiloxanes, anti-aging, low surface tension, has lubricated, soft, good spreadability and emulsion stability etc. again.In addition, the PDMS-PEO block copolymer also has biocompatibility, good adaptability and low vitrification point.
Up to now, though utilize the composite existing many reports of work that prepare ordered mesoporous material between cationic/nonionic, anionic/cationic and the nonionic/non-ionic surface active agent.But, adopt PDMS-PEO also to rarely have report as the work that common template prepares highly ordered mesosize pores macromolecule/monox nanometer composite.
Summary of the invention
The object of the invention is to propose a kind of mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure, and this material is with a wide range of applications in fields such as absorption, separation and catalysis.
Another object of the present invention is to provide the preparation method of above-mentioned nano composite material.
The objective of the invention is to realize through following technical measures:
A kind of mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure; It is characterized in that: it is to adopt bi-block copolymer dimethyl silicone polymer-polyoxyethylene (PDMS-PEO) and triblock polymer polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO; P123) be the mixed structure directed agents; The phenolic resins performed polymer is the carbon source precursor body, mix, react the As-made intermediate, make through roasting again; Said As-made intermediate in its small angle X ray scattering (SAXS) collection of illustrative plates, has three
qValue is than being the diffraction maximum of 1:2:3.
Above-mentioned As-made intermediate, it has the small angle X ray scattering curve shown in a among Fig. 1.
Nitrogen adsorption/the desorption isotherm of the mesoporous polymer/monox nanometer composite of above-mentioned tool one dimension stratiform pore passage structure has the triangle hysteresis loop.
The preparation method of the mesoporous polymer/monox nanometer composite of above-mentioned tool one dimension stratiform pore passage structure; It is characterized in that: with bi-block copolymer dimethyl silicone polymer-polyoxyethylene (PDMS-PEO) and triblock polymer polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO; P123) solution; Phenolic resins performed polymer solution mixes, the oven dry reaction, makes the mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure again through roasting; Said drying time is 20～30h, and temperature is 80～100 ℃.
The solution of above-mentioned PDMS-PEO and P123 is PDMS-PEO and P123 to be dissolved in the solvent make, and above-mentioned phenolic resins performed polymer solution is the phenolic resins performed polymer to be dissolved in the solvent make; Said solvent can be toluene, absolute ethyl alcohol, THF (oxolane) etc., most preferably adopts THF as solvent.
PDMS-PEO block copolymer of the present invention is preferably
M w =3012, DMS
32-EO
20PDMS-PEO; PEO-PPOX of the present invention-PEO (PEO-PPO-PEO), its
M w=5800, EO
20-PO
70-EO
20, trade name P123; Be the commercially available prod.
Above-mentioned carbon source precursor phenolic resins performed polymer Resol, molecular weight is 400<
M w <500, its cross-linked network is following:
The phenolic resins structural representation
The preparation of phenolic resins performed polymer solution of the present invention: be in 40～42 ℃ of fusions with 0.61g phenol; Under this temperature, add 0.13 g, the 20 wt % NaOH aqueous solution and stir 10 min; Add 1.05 g 37wt % formalins, be warming up to 70～75 ℃ of reaction 1h, reduce to room temperature; Using the pH value of 0.6mol/L HCl solution regulator solution is 7.0, is lower than 50 ℃ of vacuum decompression dehydration 1～2h; The thick liquid that obtains is dissolved in the THF solution for later use that is made into 20 wt% phenolic resins performed polymers among the THF.
Above-mentioned roasting preferably, is the mesoporous polymer/monox nanometer composite that above-mentioned As-made intermediate is obtained tool one dimension stratiform pore passage structure at 300 ~ 400 ℃ of roasting 2 ~ 4h.
Further preferably, the mass percentage concentration of the THF solution of above-mentioned phenolic resins performed polymer is 15 ~ 40wt%, and preferred concentration is 20wt%; In the THF solution of PDMS-PEO and P123, the mass percentage concentration of PDMS-PEO and P123 is 2 ~ 5wt%, and the preferred mass percentage composition is 3.2wt%.
The mass ratio of above-mentioned template PDMS-PEO, P123 and carbon source precursor body Resol is (0.8 ~ 1.1): (0.8 ~ 1.1): (2.5 ~ 3.5); Being preferably mass ratio is 1:1:3.
Specifically, the preparation method of the mesoporous polymer/monox nanometer composite of above-mentioned tool one dimension stratiform pore passage structure induces self assembly (EISA) method to make through solvent evaporates, specifically carries out as follows:
1. P123 and PDMS-PEO are dissolved among the THF, 38 ~ 45 ℃ are stirred the solution that 8 ~ 15 min obtain homogeneous transparent, and the THF solution, stirring 0.3 ~ 0.7 h that add phenolic resins performed polymer Resol then obtain uniform solution; The mass ratio of above-mentioned substance is PDMS-PEO:P123:Resol=0.8 ~ 1.1:0.8 ~ 1.1:2.5 ~ 3.5, and preferred mass is than being PDMS-PEO:P123:Resol=1:1:3; The mass percentage concentration of the THF solution of phenolic resins performed polymer is 15 ~ 40wt%, and preferred concentration is 20wt%, and in the THF solution of PDMS-PEO and P123, the mass percentage concentration of PDMS-PEO and P123 is 2 ~ 5wt%, and the preferred mass percentage composition is 3.2wt%; Above-mentioned solution is transferred in the culture dish, and 5～8 h that volatilize under the room temperature place 24h in 100 ℃ of baking ovens with culture dish again, obtain transparent orange-yellow thin-film material.Above-mentioned material is scraped from culture dish, and grind into powder obtains the As-made sample;
2. place tube furnace under the nitrogen gas protection, to carry out roasting in above-mentioned As-made sample, 300 ~ 400 ℃ of roasting 2 ~ 4h obtain the mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure, and programming rate is 5 ℃/min.
More particularly, the preparation method of the mesoporous polymer/monox nanometer composite of above-mentioned tool one dimension stratiform pore passage structure:
1. 0.5 g P123 and 0.5 g PDMS-PEO are dissolved in the 30.0 g oxolanes (THF), 40 ℃ are stirred 10 min, obtain the solution of transparent and homogeneous.Add then 7.5g 20 wt % phenolic resins performed polymers (
M w<500) THF solution stirs 0.5h and obtains uniform solution.Above-mentioned solution is transferred in the culture dish, and 5～8 h that volatilize under the room temperature place 24h in 100 ℃ of baking ovens with culture dish again, obtain transparent orange-yellow thin-film material.Above-mentioned material is scraped from culture dish, and grind into powder obtains the As-made sample.
2. place tube furnace under 350 ℃ of nitrogen gas protections, to carry out mesoporous polymer/monox nanometer composite that roasting 3h makes tool one dimension stratiform pore passage structure in the As-made sample, programming rate is 5 ℃/min.Gained mesoporous polymer/monox nanometer composite sample is labeled as MP-PS-350N.
Adjustment in the present invention such as each material variety and usage ratio, technological parameter, situation such as the mesoporous polymer of prepared tool one dimension stratiform pore passage structure/monox nanometer composite degree of order difference, skeleton contraction are different.
The present invention has following beneficial effect:
1, the thermally-stabilised scope of the layer structure of the mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure of the present invention is at 300 ~ 380 ℃, and interlamellar spacing is in 8 ~ 15nm scope, and specific area, pore volume and aperture be 500 ~ 900 m respectively
2/ g, 0.40 ~ 0.58 cm
3/ g and 4.5 ~ 5.6 nm.Mesoporous polymer/monox nanometer the composite of tool one dimension stratiform pore passage structure of the present invention is particularly suitable for fields such as low-k coating, film separation, sensor, optical material.
2, the hydrophobicity of PDMS segment is very strong in the PDMS-PEO block copolymer, carries out when composite with P123, can obviously increase the hydrophobic inner core of P123, thus the aperture that effectively increases the gained mesoporous material; On the other hand; PDMS-PEO again can be as the silicon source; Formed mesoporous material is in high-temperature roasting template agent removing process; Inorganic PDMS segment is converted into silica rigidity component, has effectively overcome shortcomings such as skeleton shrinks seriously in the simple organic system carbonisation, the aperture is little, specific area is low; Thereby can silica be incorporated in the meso-porous carbon material system through one-step method; Need not introduce expensive silane reagent; And avoided traditional sol-gel process; Simplify the preparation process of mesoporous polymer/monox nanometer composite greatly, thereby hewed out the synthetic route of a novel economical rationality, workable mesoporous polymer/monox nanometer composite.Prepared mesoporous polymer/monox nanometer composite has stable stratiform pore passage structure, big aperture and specific area, has broad application prospects in fields such as low-k coating, film separation, sensor, optical materials.
Description of drawings
Fig. 1 is small angle X ray scattering (SAXS) collection of illustrative plates of layered mesoporous macromolecule/monox nanometer composite sample: (a) As-made sample, (b) sample (MP-CS-350N) that obtains of the following 350 ℃ of roastings of nitrogen atmosphere;
Fig. 2 is transmission electron microscope (TEM) image of layered mesoporous macromolecule/monox nanometer composite sample MP-CS-350N;
Fig. 3 be layered mesoporous macromolecule/monox nanometer composite MP-CS-350N sample nitrogen adsorption/desorption isotherm (A) and pore size distribution curve (B).
The specific embodiment
Below in conjunction with accompanying drawing the present invention is further specified; But following explanation is not to limit of the present invention; Any to distortion of the present invention and change, only otherwise break away from spirit of the present invention, all should belong to the defined scope of accompanying claims of the present invention.
Embodiment 1Synthesizing of phenolic resins performed polymer
With 0.61g phenol in 40～42 ℃ of fusions; Under this temperature, add 0.13 g, the 20 wt % NaOH aqueous solution and stir 10 min; Add 1.05 g 37wt % formalins, be warming up to 70～75 ℃ of reaction 1h, reduce to room temperature; Using the pH value of 0.6mol/L HCl solution regulator solution is 7.0, is lower than 50 ℃ of vacuum decompression dehydration 1～2h.The thick liquid that obtains is dissolved in is made into 20 wt% solution for later use among the THF.
Embodiment 2The preparation of As-made sample
0.5 g P123 and 0.5 g PDMS-PEO are dissolved in the 30.0 g oxolanes (THF), and 40 ℃ are stirred 10 min, obtain the solution of transparent and homogeneous.Add then 7.5 g, 20 wt % phenolic resins performed polymers (
M w<500) THF solution stirs 0.5h and obtains uniform solution.Above-mentioned solution is transferred in the culture dish, and 5～8 h that volatilize under the room temperature place 24h in 100 ℃ of baking ovens with culture dish again, obtain transparent orange-yellow thin-film material.Above-mentioned material is scraped from culture dish, and grind into powder obtains the As-made sample.
Triblock copolymer P123 among this embodiment (
M w=5800, EO
20-PO
70-EO
20) purchase company in Aldrich, PDMS-PEO (
M w=3012, DMS
32-EO
20) purchase Mai Ruier chemical technology Co., Ltd in Shenzhen, other reagent is purchased the chemical reagents corporation in Shanghai, does not all further handle before all reagent use.
Embodiment 3The preparation of the mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure
Place tube furnace under 350 ℃ of nitrogen gas protections, to carry out roasting 3h in the As-made sample, programming rate is 5 ℃/min.Gained mesoporous polymer/monox nanometer composite sample is labeled as MP-PS-350N.
Embodiment 4Adopt the German Brooker Nanostar U of company small angle X ray scattering appearance (CuK α) to measure above-mentioned gained sample is carried out small angle X ray scattering (SAXS) mensuration, pipe is pressed 40 kV, pipe stream 35 mA, and be 30 min writing time.Gained SAXS is as shown in Figure 1.Can find out that by Fig. 1 (a) the SAXS spectrogram of As-made sample is at 0.52,0.99 and 1.54 nm
-13 diffraction maximums clearly, these 3 diffraction maximums appear in the place
qValue is referred to layered mesoporous result's crystal face diffraction maximum than being 1:2:3.After the roasting, the SAXS spectrogram of gained sample MP-PS-350N also can be observed two obvious diffraction peaks under 350 ℃ of nitrogen protections, the 3rd diffraction maximum is fainter, through calculating 3 diffraction maximums
qValue is 1:2:3 than also.This explanation layer structure meso-hole structure after through 350 ℃ of roastings still keeps.
Embodiment 5Adopt Japanese JEOL JEM2011 type high-resolution-ration transmission electric-lens (TEM) that the structure of above-mentioned gained sample MP-PS-350N is characterized, accelerating potential is 200 kV.The gained result is as shown in Figure 2.Can be found out that by Fig. 2 sample MP-PS-350N has tangible layered mesoporous structure, black region is SiO among the figure
2Composition, bright zone are that surfactant is removed formed lamellar spacing, back, and interlamellar spacing is 10.5nm.
Embodiment 6Adopt Micromeritics Tristar 3000 absorption appearance that above-mentioned gained sample MP-PS-350N is carried out nitrogen adsorption/desorption performance test.Nitrogen adsorption/desorption isotherm obtains under 77 K conditions.Before the test, sample is no less than 6 h in 200 ℃ of degassings in advance under vacuum condition.The specific area of sample (
S BET ) adopt the BET method, calculate according to relative pressure adsorpting data in the 0.04-0.2 scope; Pore volume (
V t ) and the aperture (
D) adopt the BJH Model Calculation by thermoisopleth absorption branch, wherein pore volume calculates with the adsorbance at relative pressure P/P0=0.992 place.Nitrogen adsorption/the desorption isotherm of MP-PS-350N (A) and pore size distribution curve (B) are as shown in Figure 3.Can find out that by Fig. 3 (A) a tangible broad triangle hysteresis loop in relative pressure 0.4-0.8 scope, occurs, this is the adsorpting characteristic of layered mesoporous structure, has proved that further institute's synthetic sample has layer structure.Specific area, pore volume and the aperture of the mesoporous stratified material MP-PS-350N of gained are respectively 645 m
2/ g, 0.49 cm
3/ g and 4.9 nm.
Claims (10)
1. mesoporous polymer/monox nanometer the composite of a tool one dimension stratiform pore passage structure; It is characterized in that: it is to adopt bi-block copolymer dimethyl silicone polymer-polyoxyethylene (PDMS-PEO) and triblock polymer polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO; P123) be the mixed structure directed agents; The phenolic resins performed polymer is the carbon source precursor body, mix, react the As-made intermediate, make through roasting again; Said As-made intermediate in its small angle X ray scattering (SAXS) collection of illustrative plates, has three
qValue is than being the diffraction maximum of 1:2:3.
2. nano composite material as claimed in claim 1 is characterized in that: said As-made intermediate, it has the small angle X ray scattering curve shown in a among Fig. 1.
3. according to claim 1 or claim 2 nano composite material, it is characterized in that: the nitrogen adsorption/desorption isotherm of the mesoporous polymer/monox nanometer composite of said tool one dimension stratiform pore passage structure has the triangle hysteresis loop.
4. like the preparation method of the mesoporous polymer/monox nanometer composite of each said tool one dimension stratiform pore passage structure of claim 1～3; It is characterized in that: with bi-block copolymer dimethyl silicone polymer-polyoxyethylene (PDMS-PEO) and triblock polymer polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO; P123) THF solution; Mix, dry reaction with the THF solution of phenolic resins performed polymer, make the mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure again through roasting; Said drying time is 20～30h, and temperature is 80～100 ℃.
5. preparation method as claimed in claim 4 is characterized in that: said PDMS-PEO block copolymer, for
M w=3012, DMS
32-EO
20PDMS-PEO.
6. like claim 4 or 5 described preparation methods, it is characterized in that: said roasting is at 300 ~ 400 ℃ of roasting 2 ~ 4h with said As-made intermediate.
7. like claim 4,5 or 6 described preparation methods, it is characterized in that: the mass percentage concentration of the THF solution of said phenolic resins performed polymer is 15 ~ 40wt%; In the THF solution of PDMS-PEO and P123, the mass percentage concentration of PDMS-PEO and P123 is 2 ~ 5wt%.
8. like claim 4,5,6 or 7 described preparation methods, it is characterized in that: the mass ratio of said PDMS-PEO, P123 and Resol is (0.8 ~ 1.1): (0.8 ~ 1.1): (2.5 ~ 3.5).
9. method as claimed in claim 4, carry out as follows:
P123 and PDMS-PEO are dissolved among the THF, and 38 ~ 45 ℃ are stirred the solution that 8 ~ 15 min obtain homogeneous transparent, and the THF solution, stirring 0.3 ~ 0.7 h that add phenolic resins performed polymer Resol then obtain uniform solution; The mass ratio of above-mentioned substance is PDMS-PEO:P123:Resol=1:1:3; The mass percentage concentration of the THF solution of phenolic resins performed polymer is 20wt%, and in the THF solution of PDMS-PEO and P123, the mass percentage concentration of PDMS-PEO and P123 is 3.2wt%; Above-mentioned solution is transferred in the culture dish, and 5～8 h that volatilize under the room temperature place 24h in 100 ℃ of baking ovens with culture dish again, obtain transparent orange-yellow thin-film material; Above-mentioned material is scraped from culture dish, and grind into powder obtains the As-made sample;
Place tube furnace under the nitrogen gas protection, to carry out roasting in above-mentioned As-made sample, 300 ~ 400 ℃ of roasting 2 ~ 4h obtain the mesoporous polymer/monox nanometer composite of tool one dimension stratiform pore passage structure, and programming rate is 5 ℃/min.
10. method as claimed in claim 4, carry out as follows:
0.5 g P123 and 0.5 g PDMS-PEO are dissolved in the 30.0 g oxolanes (THF), and 40 ℃ are stirred 10 min, obtain the solution of transparent and homogeneous;
The THF solution that adds 7.5g 20 wt % phenolic resins performed polymers then stirs 0.5h and obtains uniform solution;
Above-mentioned solution is transferred in the culture dish, and 5～8 h that volatilize under the room temperature place 24h in 100 ℃ of baking ovens with culture dish again, obtain transparent orange-yellow thin-film material; Above-mentioned material is scraped from culture dish, and grind into powder obtains the As-made sample;
Place tube furnace under 350 ℃ of nitrogen gas protections, to carry out mesoporous polymer/monox nanometer composite that roasting 3h makes tool one dimension stratiform pore passage structure in the As-made sample, programming rate is 5 ℃/min.
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| CN103041754A (en) * | 2013-01-30 | 2013-04-17 | 同济大学 | Polymer micelle modified by nano copper oxide and preparation method of polymer micelle |
| CN110655330A (en) * | 2019-10-29 | 2020-01-07 | 湘潭大学 | Preparation method of phenolic resin ordered mesoporous film based on rapid thermal treatment |
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| CN103041754A (en) * | 2013-01-30 | 2013-04-17 | 同济大学 | Polymer micelle modified by nano copper oxide and preparation method of polymer micelle |
| CN103041754B (en) * | 2013-01-30 | 2015-06-03 | 同济大学 | Polymer micelle modified by nano copper oxide and preparation method of polymer micelle |
| CN110655330A (en) * | 2019-10-29 | 2020-01-07 | 湘潭大学 | Preparation method of phenolic resin ordered mesoporous film based on rapid thermal treatment |
| CN110655330B (en) * | 2019-10-29 | 2021-08-20 | 湘潭大学 | Preparation method of phenolic resin ordered mesoporous film based on rapid thermal treatment |
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