USH409H - Synthesis of cadmium sulfide using the laser-induced reaction of dialkylcadmium and organosulfur compounds - Google Patents
Synthesis of cadmium sulfide using the laser-induced reaction of dialkylcadmium and organosulfur compounds Download PDFInfo
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- USH409H USH409H US07/067,770 US6777087A USH409H US H409 H USH409 H US H409H US 6777087 A US6777087 A US 6777087A US H409 H USH409 H US H409H
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- torr
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- dialkylcadmium
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 25
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 23
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 title claims description 3
- 238000003786 synthesis reaction Methods 0.000 title claims description 3
- 150000002898 organic sulfur compounds Chemical class 0.000 title description 2
- 239000000376 reactant Substances 0.000 claims abstract description 22
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 230000005855 radiation Effects 0.000 claims abstract description 12
- 230000005284 excitation Effects 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims 8
- VQNPSCRXHSIJTH-UHFFFAOYSA-N cadmium(2+);carbanide Chemical compound [CH3-].[CH3-].[Cd+2] VQNPSCRXHSIJTH-UHFFFAOYSA-N 0.000 claims 3
- 230000001678 irradiating effect Effects 0.000 claims 2
- 239000007787 solid Substances 0.000 claims 2
- 239000000203 mixture Substances 0.000 abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract 1
- 229910018503 SF6 Inorganic materials 0.000 description 10
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 10
- 238000002329 infrared spectrum Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 230000001427 coherent effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 108010067216 glycyl-glycyl-glycine Proteins 0.000 description 2
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- JLLMPOYODONDTH-UHFFFAOYSA-N selanylidenezirconium Chemical compound [Se].[Zr] JLLMPOYODONDTH-UHFFFAOYSA-N 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- GZXOHHPYODFEGO-UHFFFAOYSA-N triglycine sulfate Chemical compound NCC(O)=O.NCC(O)=O.NCC(O)=O.OS(O)(=O)=O GZXOHHPYODFEGO-UHFFFAOYSA-N 0.000 description 2
- 238000001845 vibrational spectrum Methods 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
Definitions
- Cadmium sulfide single crystal is used as a UV detector and in combination with other materials indium antimony (InSb) as a detector for UV and IR detectors.
- the final product material must meet a very strict set of specifications with respect to spectral transmission, mobility, resistivity, and detector lifetime.
- the single crystals are prepared using a "proprietary" process which involves chemical vapor deposition by Eagle Picher Laboratories, who is at present the single supplier. It is concluded that the characteristics of the single crystal are drastically affected by the purity of the cadmium sulfide powder used as a precursor to the single crystal. The basis for this conclusion is supported by P. D. Fochs et al, Report No. AE-1-G.1453, Clevite Corporation, Report No. FTD-TT-65-555, General Electric Company, Report No. SR-2,65gc-03 136, and Bell and Howell Research center, Technical Report AF 33-615-276.
- Hydrogen sulfide is known to be acidic in solution; however, a reaction in liquid solution to yield cadmium sulfide is not desired to be pursued since the required level of purity of the finished product by this route cannot be achieved.
- an object of this invention is to provide a laser-induced reaction to precisely produce sulfur to react with cadmium from an organocadmium compound selected from a dialkylcadmium compound to yield a high purity thermodynamically stable cadmium sulfide.
- a further object of this invention is to provide a laser-induced chemical reaction between a dialkylsulfide and a dialkylcadmium compound to yield high purity thermodynamically stable cadmium sulfide.
- a further object of this invention is to provide a laser-induced chemical reaction wherein the compound SF 6 is mixed with a dialkylsulfide compound and a dialkylcadmium compound wherein the compound SF 6 has a fundamental which allows the excitation to occur by absorption of laser energy followed by collisional transfer to effect a higher yield of high purity thermodynamically stable cadmium sulfide.
- a method of synthesis comprises a laser-induced chemical reaction between a first reactant of a dialkylcadmium and a second reactant of a dialkylsulfide to form high purity cadmium sulfide.
- the reactants are induced to react by laser irradiation wherein the reaction is carried out in a stainless steel cell (5 ⁇ 10 cm) equipped with O-ring seals for securing windows (5 cm diameter) onto the cells.
- Potassium chloride windows are used on the short pathlength (5 cm) for recording the infrared spectra.
- a zirconium selenium (ZrSe) window is used to transmit the incident infrared radiation; however, since only about 65% of the incident radiation is transmitted through the ZrSe window the laser power available to the sample must be adjusted accordingly.
- Infrared laser radiation in the range of 10.4 or 9.4 micrometers is provided by a Coherent Radiation Laboratories model 41 continuous-wave CO 2 laser. In single line operation, output powers between 10 and 150 W/cm 2 are obtained by variation of the CO 2 -N 2 -He gas mixture in the laser.
- Dimethylsulfide is irradiated at R(18) of (00°1-10°0) for 5 seconds at 100 W/cm 2 .
- the products formed are methane, ethane, and sulfur.
- a mixture of a dialkylsulfide, (CH 3 ) 2 S, and a dialkylcadmium, (CH 3 ) 2 Cd is irradiated at R(18) of (00°1-10°0), 979 cm -1 for a total of 5 seconds at 100 W/cm 2 .
- CdS is formed on the windows and methane and ethane are other products that remain in the gaseous mixture.
- a higher yield of CdS is obtained when SF 6 is added to the mixture of the reactants. Excitation of the SF 6 , (CH 3 ) 2 S, and (CH 3 ) 2 Cd mixture occurs using P(20) of (00°1-10°0) at 944 cm -1 for 5 seconds at 100 W/cm 2 .
- Using SF 6 results in an enhanced reaction of (CH 3 ) 2 S and (CH 3 ) 2 Cd to produce a higher yield of high purity CdS.
- FIG. 1 depicts a typical experimental setup for laser-induced chemical reaction and monitoring the induced reaction.
- FIG. 2 depicts infrared spectra curves A, B, and C which respectively represent (CH 3 ) 2 Cd at 33 torr, (CH 3 ) 2 Cd and (CH 3 ) 2 S mixed to form a mixture at 100 torr, and the mixture of (CH 3 ) 2 Cd and (CH 3 ) 2 S after irradiation.
- FIG. 3 depicts infrared spectra curves A, B, and C representing the result of the laser-induced reaction of (CH 3 ) 2 S and (CH 3 ) 2 Cd as enhanced with the sensitizer SF 6 .
- An organosulfur compound is used as a reactant to precisely produce sulfur which reacts with cadmium released from another reactant, a dialkylcadmium, to produce high purity cadmium sulfide.
- Sample handling is accomplished using standard vacuum line techniques.
- the reactants are gaseous products, and the gas phase reaction which is induced by infrared laser radiation is carried out in stainless steel cells (5 ⁇ 10 cm) equipped with O-ring seals for securing windows (5 cm diameter) onto the cells.
- Potassium chloride windows are used on the short pathlength (5 cm) for recording the infrared spectra.
- a zirconium selenium (ZrSe) window is used to transmit the incident infrared radiation; however, since only about 64% of the incident radiation is transmitted through the ZrSe window the laser power available to the sample must be adjusted accordingly.
- Infrared spectra are recorded on a Mattson Sirius 100 interferometer equipped with a water-cooled carborundum source, iris aperture, potassium bromide (KBr) beamsplitter, and triglycine sulfate (TGS) detector. Interferograms are transformed after applying a triangular apodization function with an effective spectral resolution of 1.0 cm -1 . This resolution is sufficient to allow unequivocal identification of all the products as well as to monitor the decrease of the starting material from its infrared absorption bands.
- Infrared laser radiation in the range of 10.4 or 9.4 micrometers is provided by a Coherent Radiation Laboratories model 41 continous-wave CO 2 laser. The exact laser frequencies are verified using an Optical Engineering CO 2 spectrum analyzer. In single line operation, output powers between 10 and 150 W/cm 2 are obtained by variation of the CO 2 -N 2 -He gas mixture in the laser. The beam size is measured from burn patterns and is found to be approximately circular with a 4 mm diameter.
- Dimethylsulfide is admitted to the reaction cell and decomposed following irradiation at R(18) of (00°1-10°0) for 5 seconds at 100 watts/centimeters square (100 W/cm 2 ).
- the products formed are methane, ethene, and sulfur.
- a mixture of the dialkylsulfide, (CH 3 ) 2 S, and the dialkylcadmium, (CH 3 ) 2 Cd in the reaction cell is irradiated at R(18) of (00°1-10°0), 979 cm -1 for a total of 5 seconds at 100 W/cm 2 .
- CdS is formed on the window and methane and ethane remains in the gaseous mixture.
- Sulfur hexafluoride is mixed with (CH 3 ) 2 S and (CH 3 ) 2 Cd in the reaction cell as an intensifier.
- SF 6 has a fundamental at 944 cm -1 which allows the excitation to occur by absorption of energy followed by collisional transfer to other molecules. Excitation occurred using P(20) of (00°1-10°0) at 944 cm -1 for 5 seconds at 100 W/cm 2 .
- the result of using SF 6 is the enhanced reaction of the excited elements of said (CH 3 ) 2 S and (CH 3 ) 2 Cd to produce CdS in larger quantities.
- Table I identifies the frequencies used to identify the products depicted by the infrared spectra curves A, B, and C of FIG. 2.
- Table II below identifies the vibrational frequencies (cm -1 ) used to identify the reactants and reaction products of (CH 3 ) 2 S, (CH 3 ) 2 Cd, and SF 6 .
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
Cadmium sulfide is formed successfully from the laser-induced chemical reion between a first reactant of a dialkylcadmium and a second reactant of a dialkylsulfide. Infrared laser radiation in the range of 10.4 or 9.4 micrometers is provided by a continuous-wave CO2 laser. In single line operation, output powers between 10 and 150 watts/centimeters square (W/cm2) are obtained by variation of the CO2 -N2 -He gas mixture in the laser. The process procedure and sample handling is accomplished using standard vacuum line techniques. The irradiation of dimethylsulfide at R(18) of (00°1-10°0) for 5 seconds at 100 W/cm2 produced the products methane, ethane, and sulfur. A mixture of a dialkylsulfide (CH3)2 S, and a dialkylcadmium (CH3)2 Cd is irradiated at R(18) of (00°1-10°0), 979 cm-1 for a total of 5 seconds at 100 W/cm2 to form CdS on the windows of the reaction cell. A higher yield of CdS is obtained when the sensitizer SR6 is added to the mixture of the reactants. Excitation of the mixture occurs using P(20) of (00°1-10° 0) at 944 cm-1 for 5 seconds at 100 W/cm2. The representative torr pressures of the reactants are for (CH3)2 Cd 33 torr combined with (CH3)2 S to total 100 torr pressure prior to irradiation. The efficiency when SF6 (6 torr) plus (CH3)2 Cd (22.4 torr) is combined with 54.5 torr of (CH3)2 S and irradiated is improved.
Description
The invention described herein may be manufactured, used, and licensed by or for the Government for governmental purposes without the payment to me of any royalties thereon.
Cadmium sulfide single crystal is used as a UV detector and in combination with other materials indium antimony (InSb) as a detector for UV and IR detectors. The final product material must meet a very strict set of specifications with respect to spectral transmission, mobility, resistivity, and detector lifetime. The single crystals are prepared using a "proprietary" process which involves chemical vapor deposition by Eagle Picher Laboratories, who is at present the single supplier. It is concluded that the characteristics of the single crystal are drastically affected by the purity of the cadmium sulfide powder used as a precursor to the single crystal. The basis for this conclusion is supported by P. D. Fochs et al, Report No. AE-1-G.1453, Clevite Corporation, Report No. FTD-TT-65-555, General Electric Company, Report No. SR-2,65gc-03 136, and Bell and Howell Research center, Technical Report AF 33-615-276.
Because of the high priority and importance of high purity of precursor material for a single crystal product, a variety of studies have been conducted over the past twenty years with the objective of perfecting a process which would produce purer starting material for ultimate growth of single crystals with specific properties. Predominant leaders in this area include Eagle Picher Laboratories and the Clevite Corporation Research Laboratory. The synthetic work for cadmium sulfide performed by these companies involved the chemical reaction of the elements with thermal activation as necessary.
Hydrogen sulfide is known to be acidic in solution; however, a reaction in liquid solution to yield cadmium sulfide is not desired to be pursued since the required level of purity of the finished product by this route cannot be achieved.
A laser-induced chemical reaction to yield high purity cadmium sulfide is worthy of consideration and further investigation; therefore, an object of this invention is to provide a laser-induced reaction to precisely produce sulfur to react with cadmium from an organocadmium compound selected from a dialkylcadmium compound to yield a high purity thermodynamically stable cadmium sulfide.
A further object of this invention is to provide a laser-induced chemical reaction between a dialkylsulfide and a dialkylcadmium compound to yield high purity thermodynamically stable cadmium sulfide.
Still, a further object of this invention is to provide a laser-induced chemical reaction wherein the compound SF6 is mixed with a dialkylsulfide compound and a dialkylcadmium compound wherein the compound SF6 has a fundamental which allows the excitation to occur by absorption of laser energy followed by collisional transfer to effect a higher yield of high purity thermodynamically stable cadmium sulfide.
A method of synthesis comprises a laser-induced chemical reaction between a first reactant of a dialkylcadmium and a second reactant of a dialkylsulfide to form high purity cadmium sulfide. The reactants are induced to react by laser irradiation wherein the reaction is carried out in a stainless steel cell (5×10 cm) equipped with O-ring seals for securing windows (5 cm diameter) onto the cells. Potassium chloride windows are used on the short pathlength (5 cm) for recording the infrared spectra. A zirconium selenium (ZrSe) window is used to transmit the incident infrared radiation; however, since only about 65% of the incident radiation is transmitted through the ZrSe window the laser power available to the sample must be adjusted accordingly.
Infrared laser radiation in the range of 10.4 or 9.4 micrometers is provided by a Coherent Radiation Laboratories model 41 continuous-wave CO2 laser. In single line operation, output powers between 10 and 150 W/cm2 are obtained by variation of the CO2 -N2 -He gas mixture in the laser.
Dimethylsulfide is irradiated at R(18) of (00°1-10°0) for 5 seconds at 100 W/cm2. The products formed are methane, ethane, and sulfur.
A mixture of a dialkylsulfide, (CH3)2 S, and a dialkylcadmium, (CH3)2 Cd is irradiated at R(18) of (00°1-10°0), 979 cm-1 for a total of 5 seconds at 100 W/cm2. CdS is formed on the windows and methane and ethane are other products that remain in the gaseous mixture. A higher yield of CdS is obtained when SF6 is added to the mixture of the reactants. Excitation of the SF6, (CH3)2 S, and (CH3)2 Cd mixture occurs using P(20) of (00°1-10°0) at 944 cm-1 for 5 seconds at 100 W/cm2. Using SF6 results in an enhanced reaction of (CH3)2 S and (CH3)2 Cd to produce a higher yield of high purity CdS.
FIG. 1 depicts a typical experimental setup for laser-induced chemical reaction and monitoring the induced reaction.
FIG. 2 depicts infrared spectra curves A, B, and C which respectively represent (CH3)2 Cd at 33 torr, (CH3)2 Cd and (CH3)2 S mixed to form a mixture at 100 torr, and the mixture of (CH3)2 Cd and (CH3)2 S after irradiation.
FIG. 3 depicts infrared spectra curves A, B, and C representing the result of the laser-induced reaction of (CH3)2 S and (CH3)2 Cd as enhanced with the sensitizer SF6.
The preparation of cadmium sulfide powder using laser photochemistry is achieved by employing the typical setup depicted in FIG. 1 of the drawing.
An organosulfur compound is used as a reactant to precisely produce sulfur which reacts with cadmium released from another reactant, a dialkylcadmium, to produce high purity cadmium sulfide.
Sample handling is accomplished using standard vacuum line techniques. The reactants are gaseous products, and the gas phase reaction which is induced by infrared laser radiation is carried out in stainless steel cells (5×10 cm) equipped with O-ring seals for securing windows (5 cm diameter) onto the cells. Potassium chloride windows are used on the short pathlength (5 cm) for recording the infrared spectra. A zirconium selenium (ZrSe) window is used to transmit the incident infrared radiation; however, since only about 64% of the incident radiation is transmitted through the ZrSe window the laser power available to the sample must be adjusted accordingly.
Infrared spectra are recorded on a Mattson Sirius 100 interferometer equipped with a water-cooled carborundum source, iris aperture, potassium bromide (KBr) beamsplitter, and triglycine sulfate (TGS) detector. Interferograms are transformed after applying a triangular apodization function with an effective spectral resolution of 1.0 cm-1. This resolution is sufficient to allow unequivocal identification of all the products as well as to monitor the decrease of the starting material from its infrared absorption bands.
Infrared laser radiation in the range of 10.4 or 9.4 micrometers is provided by a Coherent Radiation Laboratories model 41 continous-wave CO2 laser. The exact laser frequencies are verified using an Optical Engineering CO2 spectrum analyzer. In single line operation, output powers between 10 and 150 W/cm2 are obtained by variation of the CO2 -N2 -He gas mixture in the laser. The beam size is measured from burn patterns and is found to be approximately circular with a 4 mm diameter.
Dimethylsulfide is admitted to the reaction cell and decomposed following irradiation at R(18) of (00°1-10°0) for 5 seconds at 100 watts/centimeters square (100 W/cm2). The products formed are methane, ethene, and sulfur.
A mixture of the dialkylsulfide, (CH3)2 S, and the dialkylcadmium, (CH3)2 Cd in the reaction cell is irradiated at R(18) of (00°1-10°0), 979 cm-1 for a total of 5 seconds at 100 W/cm2. CdS is formed on the window and methane and ethane remains in the gaseous mixture.
Sulfur hexafluoride is mixed with (CH3)2 S and (CH3)2 Cd in the reaction cell as an intensifier. SF6 has a fundamental at 944 cm-1 which allows the excitation to occur by absorption of energy followed by collisional transfer to other molecules. Excitation occurred using P(20) of (00°1-10°0) at 944 cm-1 for 5 seconds at 100 W/cm2. The result of using SF6 is the enhanced reaction of the excited elements of said (CH3)2 S and (CH3)2 Cd to produce CdS in larger quantities.
Table I below identifies the frequencies used to identify the products depicted by the infrared spectra curves A, B, and C of FIG. 2.
TABLE I
______________________________________
VIBRATIONAL FREQUENCIES (cm.sup.-1).sup.(a) of (CH.sub.3).sub.2 Cd,
(CH.sub.3).sub.2 S and REACTION PRODUCTS
(CH.sub.3).sub.2 Cd +
Mixture After Refer-
(CH.sub.3).sub.2 Cd
(CH.sub.3).sub.2 S
Irradiation
Identity ence
______________________________________
3016 CH.sub.4 (c)
2900 2990 2990 X,Y(b) (d)(e)
2980 2980 2980 X,Y
2973 2973 2973 X,Y
2925 2925 2925 X,Y
2918 2918 2918 X,Y
2868 2870 X,Y
2855 2855 2855 X,Y
2838
2349 2349 2349 X,Y
1457
1441
1433
1338 1338 1338 X,Y,
1326 1326 1326 X,Y
1314 1314 1314 X,Y
1305 1305 1302 X,Y
1165 1045 1045 X,Y
1025 1021 X,Y
948 Ethylene (c)
730 730
704 704
691 691
669 669
544 544 544
524 524 524
______________________________________
.sup.(a) Only the frequencies of major bands are given
(b) X = (CH.sub.3).sub.2 Cd; Y = (CH.sub.3 ).sub.2 S
(c) Herzberg, G., Infrared and Raman Spectra (Van Nostrand Reinhold, New
York, 1945), First Edition.
(d) Bakhe, A. M. W., J. Mol. Spectrosc. 41, 1-19 (1972).
(e) P. Groner, J. F. Sullivan, and J. R. Durig, in Vibrational Spectra an
Structures, edited by J. R. Durig (Elsevier, Amsterdam, 1986), Vol. 9,
Chap. 6.
Table II below identifies the vibrational frequencies (cm-1) used to identify the reactants and reaction products of (CH3)2 S, (CH3)2 Cd, and SF6.
TABLE II
______________________________________
VIBRATIONAL FREQUENCIES (cm.sup.-1).sup.(a) of (CH.sub.3).sub.2 S,
(CH.sub.3).sub.2 Cd and SF.sub.6 and REACTION PRODUCTS.
Mixture + After Refer-
(CH.sub.3).sub.2 Cd + SF.sub.6
(CH.sub.3).sub.2 S
Irradiation
Identity
ence
______________________________________
3016 (.9) CH.sub.4
(e)
2990 2988 (.2) X,Y(b) (d),(c)
2980 2979 (.2) X,Y
2970 2970 2969 (.2) X,Y
2958 (.2)
2951 2945 2948 (.2)
2940 2938 (.2)
2930 2927 (.2)
2916 2917 (.2)
2864
2851
2840
1558 1558 1558 (.5)
1541 1541 1541 (2.9)
1532 (.4)
1521 1523 (1.3)
1507 1507 1508 (.6)
1489 (.2)
1473 (.2)
1457 1457 1457 (.2) X,Y (d),(c)
1437
1430
1362 X,Y (d),(c)
1339 1340
1314
1304 1304
945.6 945 945 SF.sub.6
(c)
930 930
724 729
711
705 704
692 691
669 669
626 626 629
614 615 614
603 603 603
544 544
527 527
______________________________________
.sup.(a) Only the frequencies of a major bands are given.
(b) X = (CH.sub.3).sub.2 Cd; Y = (CH.sub.3).sub.2 S
(c) Herzberg, G., Infrared and Raman Spectra (Van Nostrand Reinhold, New
York, 1945), First Edition.
(d) Bakhe, A. M. W. J. Mol. Spectrosc. 41, 1-19 (1972).
(e) P. Groner, J. F. Sullivan, and J. R. Durig, in Vibrational Spectra an
Structures, edited by J. R. Durig (Elsevier, Amsterdam, 1986), Vol. 9,
Chap. 6.
Claims (5)
1. A method for the synthesis of cadmium sulfide by the laser-induced chemical reaction between a first reactant selected from a dialkylcadmium compound and a second reactant selected from a dialkylsulfide compound, said method comprising:
(i) providing a stainless steel reaction cell adapted for use with vacuum line techniques and equipped with O-ring seals for securing ZrSe windows onto said reaction cell for transmitting laser radiation and for securing potassium chloride windows onto said reaction cell to achieve monitoring of said laser-induced chemical reaction including the reaction products formed;
(ii) metering said first reactant of said dialkylcadmium compound and said second reactant of said dialkylsulfide into said reaction cell to form a reaction mixture of said dialkycadmium compound in the range from about 14 to about 32 torr and of said dialkylsulfide compound in the range from about 30 to about 279 torr;
(iii) irradiating said reaction mixture with infrared laser radiation in the range of 10.4 or 9.4 micrometers as provided by a continuous-wave CO2 laser operating in a predetermined single line operation with an output power between about 10 and 150 watts per centimeter square (W/cm2) to form reaction products including a solid compound; and,
(iv) recovering said solid compound which is high purity thermodynamically stable cadmium sulfide.
2. The method of claim 1 wherein said dialkylcadmium is dimethylsulfide and wherein said reaction mixture comprises said dimethylcadmium of about 3 torr and said dimethylsulfide of about 100 torr.
3. The method of claim 1 wherein said irradiating of said reaction mixture is achieved with said predetermined single line operation at R(18) of (00°1-10°0) for about 5 seconds at 975 cm-1, said output power is 100 W/cm2, and wherein said dialkylcadmium compound is dimethylcadmium of about 33 torr and said dialkylsulfide compound is dimethylsulfide of about 100 torr which comprises said first and second reactant respectively of said reaction mixture.
4. The method of claim 1 wherein said reaction mixture additionally comprises SF6 as an intensifier which has a fundamental at 944 cm-1 to allow excitation to occur by absorption of energy followed by collisional transfer to said first reactant and to said second reactant to achieve enchanced reaction of the excited elements of said first and said reactants to produce said cadmium sulfide in higher yield.
5. The method of claim 4 wherein said reaction mixture comprises said SF6 of about 6 torr, said first reactant of said dialkylcadmium is dimethylcadmium of about 22.4 torr, said second reactant of said dialkylsulfide is dimethylsulfide of about 54.5 torr, and wherein said irradiation of said reaction mixture is achieved with said predetermined single line operation at P(20) of (00°1-10°0) for about 5 seconds at said output power which is 100 W/cm2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/067,770 USH409H (en) | 1987-06-29 | 1987-06-29 | Synthesis of cadmium sulfide using the laser-induced reaction of dialkylcadmium and organosulfur compounds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/067,770 USH409H (en) | 1987-06-29 | 1987-06-29 | Synthesis of cadmium sulfide using the laser-induced reaction of dialkylcadmium and organosulfur compounds |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| USH409H true USH409H (en) | 1988-01-05 |
Family
ID=22078302
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US07/067,770 Abandoned USH409H (en) | 1987-06-29 | 1987-06-29 | Synthesis of cadmium sulfide using the laser-induced reaction of dialkylcadmium and organosulfur compounds |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | USH409H (en) |
-
1987
- 1987-06-29 US US07/067,770 patent/USH409H/en not_active Abandoned
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