CN115872743B - MAX phase material with X position being pnicogen and/or chalcogen and preparation method thereof - Google Patents
MAX phase material with X position being pnicogen and/or chalcogen and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic nonmetallic materials, and relates to a MAX phase material with X-position being pnicogen and/or chalcogen and a preparation method thereof. The molecular formula of the MAX phase material with the X position being pnictogen and/or chalcogen is M 2 AX, where X is a combination of one or more of the elements in P, as, sb, S, se, te. The novel MAX phase material with the X position being the pnicogen and/or the chalcogen has unique physicochemical properties and has potential application prospect in the fields of energy storage, catalysis, electrons, thermoelectricity and the like.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic materials, and relates to a MAX phase material with X-position being pnicogen and/or chalcogen and a preparation method thereof.
Background
MAThe X phase is a broad class of non-Van der Waals layered solid materials, these ternary compounds have a general formula M n+1 AX n Is in a hexagonal symmetrical structure (P6) 3 And/mmc), wherein M is a transition metal, A is mainly a main group element, X is C, N, B, n=1-3 (M.W. Barsoum et al, prog.solid State Ch 28 (1-4) (2000) 201-281). Theoretical calculation prediction shows that more than 600 MAX phases have thermodynamic stability, wherein the number of MAX phases which are successfully synthesized is more than 70. The constituent elements of the MAX phase that have been found to be present include 20 more M-bit elements, approximately 20 a-bit elements, and 3X-bit elements (C, N, B). Wherein M is n+1 X n Co-edge M of nanostructure sublayer by covalent bond 6 An X octahedral layer, wherein X element occupies an octahedral gap formed by M element; and A-bit monoatomic layer and M n+1 X n The interaction force between the nanostructure sub-layers is weak, and the nanostructure sub-layers are in an approximate metal bond state. By virtue of its unique covalent M 6 The MAX phase shows the composite properties of metal and ceramic in an alternating arrangement of X octahedra and metalloid a layers: these MAX's generally combine the light weight, high strength, oxidation resistance, creep resistance and good thermal stability of ceramics with the high electrical conductivity, high thermal conductivity, relative flexibility of metals and good damage tolerance, high temperature plasticity and workability of metals (J. Gonzalez-Julian et al, J AM chem. Soc.104 (2) (2021) 659-690). Recent studies have also found that MAX phase has low irradiation activity and good material connection properties (c.wang et al, nat.com., 2019,10,622&Zhou et al, carbon,2016,102,106-115). Therefore, most of the research on the corresponding application field of MAX is mainly focused on the direction of high-safety structural materials including high-temperature electrodes, high-speed rail pantographs, nuclear fuel cladding tubes and the like, and relatively less research is conducted on the application field of MAX phase functionalization.
The chemical and structural diversity of the MAX phase is critical to optimizing the performance of future applications thereof (m.sokol et al., trends in chem.1 (2) (2019) 210-223), and how to utilize the chemical diversity of the MAX phase to design and regulate the element composition and the electron cloud structure of the MAX phase, obtain the MAX phase with brand-new physicochemical properties, and promote understanding of people on the crystal structure of the MAX phase material is always an important direction of efforts of students in the field. Many experiments prove that elements at each position in the MAX phase play a decisive role in the performance of the material. However, the X-bit elements of the MAX phase studied so far are all elements (C, N, B) with smaller atomic size, and the outermost periphery has a smaller number of charges (. Ltoreq.5). Therefore, it is necessary to extend the optional range of the X-site atoms to regulate the structure and properties of the MAX-phase material.
On the other hand, transition metal sulfide materials (TMDs) and transition metal phosphide materials (TMPs) have received much attention in recent years, and are one of the hot spots in recent years of research in materials. The transition metal sulfide is a compound MX with a sandwich-like structure 2 (M represents a transition metal in the periodic Table of elements, X represents a chalcogen such as S, se), and similarly to graphene, TMDs are also connected by Van der Waals forces, and single-layer or multi-layer TMDs can be peeled from bulk materials. TMDs exhibit different conductor characteristics, such as near-insulator (HfS 2 ) (Wang, et al 2d mate, 4.3 2017:031012), semiconductor (MoS 2 ) (Yang T H, et al adv. Funct. Mater.,2018,28 (7): 1706113), metal (NbSe) 2 ) (Cai Z, et al chem. Reviews,2018,118 (13): 6091-6133). In addition, the bandgap of TMDs semiconductor materials is also dependent on the number of layers of the material, such as MoS 2 The band gap of (a) can be raised from 1.2ev (bulk) to 1.8 to 1.9ev (monolayer) (Martella C, et al adv. Mater.,2018,30 (9): 1705615). Most TMDs materials possess three features: 1T,2H and 3R (Guo B, et al ACS App. Mater).&Interr., 2017,9 (4): 3653-3660). These three phases are not fixed and can be mutually transformed under certain specific conditions. For example molybdenum disulphide is typically present in the form of a semiconductor phase (2H), but when ion migration occurs it can be converted into a metastable metal phase (1T). Whereas transition metal phosphides differ from transition metal sulfides in that TMPs have ceramic-like physical properties while retaining metal-like electronic and magnetic properties. And their crystal structure is triangular pyramid, instead of forming a layered structure like sulfide (oyamas T, et al catalyst, today,2009,143 (1-2): 94-107). They are in the catalysis ofExcellent properties such as very high catalytic activity of phosphide Ni are exhibited in desulfurization and catalytic denitration 2 P (Oyama S T, et al, journal of catalyst, 2003,216 (1-2): 343-352), this excellent catalytic property has great relevance to the manner in which the internal pnicogen atom arrangement is electronically bound, but most transition metal phosphides do not possess an ordered layered structure (Du H, et al, nanoscales, 2018,10 (46): 21617-21624). The place of the pnicogen of MAX phase containing pnicogen synthesized by powder metallurgy is basically at the A position, and the structure formed by the pnicogen and metal element is a triangular prism. Currently, no research report on MAX phase materials with X position being phosphorus and chalcogen is available.
Disclosure of Invention
The invention aims at overcoming the defects in the prior art and provides a MAX phase material with X-position being pnicogen and/or chalcogen and a preparation method thereof.
In order to achieve the aim of the invention, the invention is realized by the following scheme:
a MAX phase material with X position being pnicogen and/or chalcogen, wherein the molecular formula of the MAX phase material with X position being pnicogen and/or chalcogen is M 2 AX, where X is a combination of one or more of the elements in P, as, sb, S, se, te.
Preferably, M 2 In the AX molecular formula, M is selected from one or a combination of a plurality of Ti, zr, hf, V, nb, ta.
Preferably, M 2 In the molecular formula of AX, A is any one or the combination of any two of S, se.
The elements at each position in the MAX phase play a decisive role in the performance of the material, and the X-position elements of the MAX phase studied so far are all elements with smaller atomic size (C, N, B). The X site of the MAX phase material provided by the invention is pnictogen and/or chalcogen, the electron cloud density of the X site atom is greatly changed compared with the existing MAX phase material, and the structure and the performance of the MAX phase material are changed to a certain degree.
When the pnictogen occupies the X position of the MAX phase material, M is formed with the metal element 6 X octahedra, therebyObtaining the metal compound with new structure of orderly lamellar arrangement of pnicogen.
whenboththeaandXsitesoftheMAXphaseareoccupiedbychalcogens,theyformacompoundsimilartometalsulfides,butunlikeTMDsmaterials,thestructurallayerswithintheMAXphasearenotconnectedbyvanderwaalsforces,butareconnectedbyM-atypemetalbondsandM-Xtypecovalentbonds,respectively,andtheMAXphasealsocomprisesthephasestructureoftwosulfides: thesulfidestructureoftheM-Alayerischaracterizedbythe2Htype,whilethesulfidestructureoftheM-Xlayerischaracterizedbythe1Ttype. The special structure can lead the A position and the X position to be the same MAX of chalcogen elements and have the properties of sulfides with different characteristics, and is expected to prepare ceramic materials with different conductive characteristics.
The novel MAX phase material with the X position being pnicogen and/or chalcogen has potential application prospect in the fields of energy storage, thermoelectricity and the like.
To achieve another object of the foregoing invention, the present invention is achieved by:
a preparation method of MAX phase material with X position being pnictogen and/or chalcogen comprises the following steps: mixing boride MAX phase material, pnictogen simple substance and/or chalcogen simple substance and/or pnictogen-containing compound and/or chalcogen-containing compound, and reacting at 800-1700 ℃ in inert atmosphere to obtain MAX phase material with pnictogen and/or chalcogen at X position.
In the synthesis process of MAX phase, it is very difficult to independently introduce pnicogen and/or chalcogen into X position, in the invention, a template substitution method is adopted, so that boride MAX phase material is used as template to exchange atoms of X position with pnicogen simple substance and/or chalcogen-containing compound, and then X position is synthesized into MAX phase of pnicogen and/or chalcogen, and the formed MAX phase has larger change of electronic structure compared with the existing MAX phase material due to the introduction of phosphorus and chalcogen in X position, thereby causing the change of physical and chemical properties of MAX phase material.
Preferably, M is selected from one or a combination of a plurality of Ti, zr, hf, V, nb, ta in the boride MAX phase material.
Preferably, in the boride MAX phase material, A is one or a combination of S, se in any proportion.
Preferably, in the boride MAX phase material, X is B.
Preferably, the pnictogen-containing compound is selected from one or more of a pnictogen-containing metal compound and a pnictogen-containing nonmetal compound.
Preferably, the chalcogen-containing compound is selected from one or more of a chalcogen-containing metal compound and a chalcogen-containing nonmetal compound.
Preferably, the molar ratio of pnictogen and/or chalcogen to boride MAX phase material is > 1.
Preferably, the reaction time is 30-120 min, and the pressure is 0-100 MPa.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides a novel MAX phase material with X position being pnictogen and/or chalcogen, the introduction of the pnictogen and chalcogen in the X position causes the electronic structure to be changed greatly compared with the existing MAX phase material, thereby causing the physical and chemical properties of the MAX phase material to be changed, and the physical and chemical properties of the MAX phase material can be regulated and controlled;
(2) The novel MAX phase material with the X position being pnicogen and/or chalcogen has unique physicochemical properties and has potential application prospect in the fields of energy storage, catalysis, electrons, thermoelectricity and the like;
(3) The invention realizes the preparation of MAX phase material with X position being pnictogen and/or chalcogen for the first time, the preparation process is simple and easy to operate, the consumption is low, and the universality is realized;
(4) The invention synthesizes the MAX phase material with X position being pnictogen and/or chalcogen by utilizing the reaction of boride MAX phase material and pnictogen simple substance and/or chalcogen simple substance and/or pnictogen-containing compound and/or chalcogen-containing compound, which is an innovation in material synthesis means and provides a brand new synthesis strategy for synthesis of other novel MAX phases;
(5) The MAX phase material with X position being pnicogen and/or chalcogen is synthesized by MAX template substitution method, which has important significance for supplementing MAX phase definition, expanding the composition types and regulating and controlling chemical properties of substances.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIGS. 1a, 1b and 1c are respectively XRD patterns and full spectrum analysis result patterns of MAX phase materials with X position being pnictogen and/or chalcogen prepared in examples 1-3 of the present invention;
FIGS. 2a, 2b and 2c are SEM images of MAX phase materials prepared according to examples 1-3 of the invention with the X position being a pnictogen and/or chalcogen, respectively;
FIGS. 3a, 3b and 3c are respectively the atomic images and lattice diffraction patterns of MAX phase materials obtained by observing that X-position is pnictogen and/or chalcogen in the preparation of the embodiment 1-3 of the present invention.
Detailed Description
The technical solution of the present invention will be further described by means of specific examples and drawings, it being understood that the specific examples described herein are only for aiding in understanding the present invention and are not intended to be limiting. Unless otherwise indicated, all materials used in the examples of the present invention are those commonly used in the art, and all methods used in the examples are those commonly used in the art.
Example 1
In this embodiment, the MAX phase material with the X position being a pnictogen and/or a chalcogen is Hf 2 SeS bulk material.
The Hf 2 The preparation method of the SeS block material comprises the following steps:
(1) Weighing scaleHf taking 2 SeB powder 10g, hfS 2 5g of powder, grinding and mixing the materials to obtain a mixture;
(2) And pressing the mixture into a tablet by using a graphite die, and then placing the tablet into a spark plasma sintering system for reaction. The reaction conditions are as follows: the reaction temperature is 1600 ℃, the heat preservation time is 20min, the pressure is 50Mpa, and the argon atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the graphite mold.
(3) And removing surface graphite paper from the obtained block, polishing the block to a mirror surface by sand paper with different mesh numbers, putting the block into a 50 ℃ oven, and taking out the block for 12 hours to obtain the block material.
And (3) detecting the block treated in the step (3) by utilizing an X-ray diffraction spectrum (XRD). By full spectrum analysis by Reitveld method (R) wp = 8.357), which successfully synthesizes Hf 2 SeS-type MAX phase material (shown in FIG. 1 a) with lattice constant ofThe small amount of hafnium oxide and hafnium boride impurities present in the powder, the former may result from oxidation of hafnium element during the preparation process, and the latter from byproducts of the substitution reaction.
The fracture cross section of the block after the treatment of step (3) was observed by Scanning Electron Microscopy (SEM), and it was found that the synthesized block grains exhibited a granular structure (see fig. 2 a). As shown in table 1, the above-mentioned speculation can be further verified by TEM-based spectroscopic analysis, the block consisting of Hf, se, S elements, wherein the ratio of atomic percentages of the elements is about 2:1:1, according with experimental design and XRD analysis. It can be clearly seen using spherical aberration correcting high resolution transmission electron microscopy that the material is substantially composed of two alternately stacked nanostructures (as in FIG. 3 a), namely Hf 2 S layer and Se atomic layer.
Table 1: analysis results of the energy spectrum of the obtained block
Example 2
In this embodiment, the MAX phase material with the X position being a pnictogen and/or a chalcogen is Zr 2 SeP bulk material.
The Zr is 2 The preparation method of the SeP block material comprises the following steps:
(1) Weighing Zr 2 SeB powder 6g, P powder 1g, and the above materials were ground and mixed to obtain a mixture.
(2) The mixture is pressed into tablets by a graphite die and then is put into a high-temperature tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1600 ℃, the heat preservation time is 120min, and the argon atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the graphite mold.
(3) The obtained block is crushed, and is put into a 50 ℃ oven to be taken out for 12 hours, thus obtaining the block material.
And (3) detecting the powder processed in the step (3) by utilizing an X-ray diffraction spectrum (XRD). By full spectrum analysis by Reitveld method (R) wp = 14.335), which successfully synthesizes Zr 2 SeP MAX phase material (fig. 1 b) has a lattice constant of a=0.3755 nm and c= 1.2559nm. The small amount of hafnium oxide impurities present in the powder may result from oxidation of the hafnium element during the preparation process.
The fracture cross section of the block after the treatment of step (3) was observed by Scanning Electron Microscopy (SEM), and it was found that the synthesized block grains exhibited a granular structure (see fig. 2 b). As shown in table 2, the above presumption can be further verified by energy spectrum analysis, the block is composed of Zr, se and P elements, wherein the atomic percentage ratio of the elements is about 2:1:1, which accords with experimental design and XRD analysis. It can be clearly seen using a spherical aberration correcting high resolution transmission electron microscope that the material is substantially composed of two alternately stacked nanostructures (as in fig. 3 b), zr 2 The P layer and the Se atomic layer. And Zr: se: P is approximately equal to 2:1:1, and can be well matched with the energy spectrum analysis result.
Table 2: analysis results of the energy spectrum of the obtained block
Example 3
In this embodiment, the MAX phase material with the X position being a pnictogen and/or a chalcogen is Zr 2 SeSe block material.
The Zr is 2 The preparation method of the SeSe block material comprises the following steps:
(1) Weighing Zr 2 SeB powder 8g, zrSe 2 5g of powder, and the above materials were ground and mixed to obtain a mixture.
(2) And pressing the mixture into a tablet by using a graphite die, and then placing the tablet into a spark plasma sintering system for reaction. The reaction conditions are as follows: the reaction temperature is 1600 ℃, the heat preservation time is 20min, the pressure is 50Mpa, and the argon atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the graphite mold.
(3) And removing surface graphite paper from the obtained block, polishing the block to a mirror surface by sand paper with different mesh numbers, putting the block into a 50 ℃ oven, and taking out the block for 12 hours to obtain the block material.
And (3) detecting the block treated in the step (3) by utilizing an X-ray diffraction spectrum (XRD). By full spectrum analysis by Reitveld method (R) wp =11.01), which successfully synthesizes Zr 2 A MAX phase material of se (fig. 1 c) with lattice constant a=0.3745 nm and c= 1.2058nm. The small amount of zirconia and zirconium boride impurities present in the powder, the former may result from oxidation of the zirconium element during the preparation process and the latter from byproducts of the substitution reaction.
The fracture cross section of the block after the treatment of step (3) was observed by Scanning Electron Microscopy (SEM), and it was found that the synthesized block grains exhibited a granular structure (see fig. 2 c). As shown in table 3, the above assumption can be further verified by spectroscopic analysis that the block is composed of Zr, se elements, wherein the atomic percent ratio of elements is about 1:1, according with experimental design and XRD analysis. It can be clearly seen using a spherical aberration correcting high resolution transmission electron microscope that the material is substantially composed of two alternately stacked nanostructures (as in fig. 3 c), zr 2 Se layer and Se atomic layer composition. And Zr: se=1:1, which can be well matched with the spectrum analysis result.
Table 3: analysis results of the energy spectrum of the obtained block
Example 4
In this embodiment, the MAX phase material with the X position being a pnictogen and/or a chalcogen is Ti 2 SeAs powder material.
The Ti is 2 The preparation method of the SeAs powder material comprises the following steps:
(1) Weighing Ti 2 SeB powder 7g, tiAs 2 2.5g of powder, and the above materials were ground and mixed to obtain a mixture.
(2) The mixture is pressed into tablets by a die and then is put into a high-temperature tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1600 ℃, the heat preservation time is 120min, and the argon atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the die.
(3) And crushing the obtained block to obtain a corresponding powder product.
Example 5
In this embodiment, the MAX phase material with the X position being a pnictogen and/or a chalcogen is Hf 2 (Se 0.5 S 0.5 )(S 0.5 Sb 0.5 ) Powder material.
The Hf 2 (Se 0.5 S 0.5 )(S 0.5 Sb 0.5 ) The preparation method of the powder material comprises the following steps:
(1) Weighing Hf 2 (Se 0.5 S 0.5 ) 8g of B powder, 1g of S powder and 4g of Sb powder, and the above materials were ground and mixed to obtain a mixture.
(2) The mixture is pressed into tablets by a die and then is put into a high-temperature tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1500 ℃, the heat preservation time is 120min, and the argon atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the die.
(3) And crushing the obtained block to obtain a corresponding powder product.
Example 6
In this embodiment, the X position is MAX of pnictogen and/or chalcogenThe phase material is (Ti 1/3 Hf 1/3 Zr 1/3 ) 2 SeS powder material.
The (Ti) 1/3 Hf 1/3 Zr 1/3 ) 2 The preparation method of the SeS powder material comprises the following steps:
(1) Weighing (Ti) 1/3 Hf 1/3 Zr 1/3 ) 2 SeB powder 8g, taS 3 4g of powder, and the above materials were ground and mixed to obtain a mixture.
(2) The mixture is pressed into tablets by a die and then is put into a tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1600 ℃, the heat preservation time is 120min, and the argon atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the die.
(3) And crushing the obtained block to obtain a corresponding powder product.
Example 7
In the present embodiment, the MAX phase material in which the X position is a pnictogen and/or chalcogen is (Hf 0.5 Zr 0.5 ) 2 Se(P 0.5 S 0.5 ) Powder material.
The (Hf) 0.5 Zr 0.5 ) 2 Se(P 0.5 S 0.5 ) The preparation method of the powder material comprises the following steps:
(1) Weighing (Hf) 0.5 Zr 0.5 ) 2 SeB powder 8g, S powder 0.6g and P powder 0.6g, and the above materials were ground and mixed to obtain a mixture.
(2) The mixture is pressed into tablets by a die and then is put into a high-temperature tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1500 ℃, the heat preservation time is 150min, and the argon atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the die.
(3) And crushing the obtained block to obtain a corresponding powder product.
In addition, the inventor also replaces the corresponding raw materials and process conditions in the previous examples 1-7 with other raw materials and process conditions described in the specification, and the results show that the MAX phase material with the X position being the pnictogen and/or chalcogen can be obtained.
Compared with the existing MAX phase material, the MAX phase material with the X position being the pnicogen and/or the chalcogen provided by the embodiment of the invention has the characteristics that the electronic structure of the material can be changed by regulating and controlling the X position element, so that the materialization property of the material is further changed, the preparation process is simple and easy to operate, and the MAX phase material has potential application prospect in the fields of energy storage, catalysis, electronics, thermoelectricity and the like.
The various aspects, embodiments, features of the invention are to be considered as illustrative in all respects and not intended to limit the invention, the scope of which is defined solely by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, and feature of the present disclosure.
In the preparation method of the invention, the sequence of each step is not limited to the listed sequence, and the sequential change of each step is also within the protection scope of the invention without the inventive labor for the person skilled in the art. Furthermore, two or more steps or actions may be performed simultaneously.
Finally, it should be noted that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention's embodiments. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions in a similar manner, and need not and cannot fully practice all of the embodiments. While these obvious variations and modifications, which come within the spirit of the invention, are within the scope of the invention, they are to be construed as being without departing from the spirit of the invention.
Claims (6)
1. A MAX phase material with X position being pnicogen and/or chalcogen is characterized in that the molecular formula of the MAX phase material with X position being pnicogen and/or chalcogen isM 2 AX, wherein X is a combination of one or more of the elements in P, as, sb, S, se, te, M is selected from a combination of one or more of Ti, zr, hf, V, nb, ta, and a is any one of S, se or a combination of both in any ratio.
2. A method for producing a MAX phase material having a pnictogen and/or chalcogen X position as claimed in claim 1, comprising the steps of: mixing boride MAX phase material, pnictogen and/or chalcogen simple substance and/or pnictogen-containing compound and/or chalcogen-containing compound, and making them react in inert atmosphere at 800-1700 deg.C so as to obtain M whose X position is pnictogen and/or chalcogen 2 AX phase material;
in the boride MAX phase material, M is selected from one or a combination of a plurality of Ti, zr, hf, V, nb, ta, and A is any one or a combination of two of S, se in any proportion.
3. The method according to claim 2, wherein the pnictogen-containing compound is one or more selected from a pnictogen-containing metal compound and a pnictogen-containing nonmetal compound.
4. The method according to claim 2, wherein the chalcogen-containing compound is one or more selected from the group consisting of a chalcogen-containing metal compound and a chalcogen-containing nonmetallic compound.
5. The method according to claim 2, wherein the molar ratio of pnictogen and/or chalcogen to boride MAX phase material is > 1.
6. The preparation method according to claim 2, wherein the reaction time is 30-120 min and the pressure is 0-100 mpa.
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