Patent
Atlas literature
Patent
US 11,692,134 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for producing an InP quantum dot precursor from a phosphorus source and an indium source, wherein a silylphosphine compound represented by the following For-mula (1) with a content of a compound represented by the following Formula (2) of 0.3 mol % or less: R R Si R R R P R Si Si R R R wherein each R is independently an alkyl group having 1 or more and 5 or less carbon atoms or an aryl group having 6 or more and 10 or less carbon atoms, H R R P R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (3) of 0.1 50 mol % or less: PH₂ Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (4) of 0.5 mol % or less: B₂ R R O R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (5) of 0.05 mol % or less: R R R R Si Si R O O R P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, a silylphosphine compound rep-resented by the Formula (1) with a content of a compound represented by the following Formula (6) of 0.05 mol % or less: R R R R Si R O Si R O O P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by Formula (1) with a content of a compound represented by the following Formula (7) of 0.2 mol % or less: R R R Si R R Si P P Si R R Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein at least one selected from the group consisting of indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate and indium oleate is used as the ndium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein an indium carboxylate with no absorption peak derived from a hydroxyl group observed in the range of 1500 cm⁻¹ or more and 1700 cm⁻¹ or less in IR spectrum is used as the indium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a reaction between the phosphorus source and the indium source is performed at a temperature in the range of 20° C. or more and 150° C. or less.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in an organic solvent.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in the presence of a trialkylphosphine.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained by the method according to claim 1 to a temperature of 200° C. or more and 350° C. or less to obtain an InP quantum dot.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained B₂ by the method according to claim 1 together with a com-pound containing an element source M (M is at least one selected from the group consisting of Be, Mg, Ca, Mn, Cu, Zn, Cd, B, Al, Ga, N, As, Sb and Bi) other than a phospho-rous source and an indium source to a temperature of 200° C. or more and 350° C. or less to obtain a composite quantum dot of In, P and M.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Production of tris(trimethylsilyl)phosphine (TMSP) as the silylphosphine compound represented by Formula (1). Degassed/dehydrated toluene (189.8 kg), triethylamine (82 kg), trimethylsilyl trifluoromethanesulfonate (149.5 kg) were combined in a reaction vessel under nitrogen, liquid temperature adjusted to 30°C, then 7.4 kg of phosphine gas was fed over 3 hours. After aging at 35°C for 4 hours, the two-layer reaction solution was separated, concentrated under reduced pressure (6.3 kPa, 70°C), and distilled (0.5 kPa, 85°C column top). 49.3 kg of main fraction (TMSP) was collected. Purity and impurity content (Formulas (2)–(7)) were measured by 31P-NMR and GC. Results: TMSP 99.6 mol%, Formula (2) 0.15 mol%, Formula (3) N.D., Formula (4) 0.08 mol%, Formula (5) N.D.
2 materials1 process step
Production of tris(trimethylsilyl)phosphine using diethyl ether as solvent (156.9 g), triethylamine (82 g), trimethylsilyl trifluoromethanesulfonate (149.5 g), and 7.4 g phosphine gas. Similar process to Production Example 1 but with different solvent. Results: TMSP 98.3 mol%, Formula (2) 0.35 mol%, Formula (3) N.D., Formula (4) 0.18 mol%, Formula (5) 0.10 mol%.
2 materials1 process step
Production of indium myristate. Degraded indium acetate was used as a model hydroxyl group-containing indium carboxylate (commercially available indium acetate stored for ~100 days). Analysis by ICP emission spectrometer was performed.
Materials described outside the worked examples.
compound of Formula (2) — mono-H silylphosphine impurity
compound of Formula (3) — H₂P-SiR₃ impurity
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
TMSP purity — Production Example 1 | 99.6 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Production Example 1 |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
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US 11,692,134 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for producing an InP quantum dot precursor from a phosphorus source and an indium source, wherein a silylphosphine compound represented by the following For-mula (1) with a content of a compound represented by the following Formula (2) of 0.3 mol % or less: R R Si R R R P R Si Si R R R wherein each R is independently an alkyl group having 1 or more and 5 or less carbon atoms or an aryl group having 6 or more and 10 or less carbon atoms, H R R P R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (3) of 0.1 50 mol % or less: PH₂ Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (4) of 0.5 mol % or less: B₂ R R O R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (5) of 0.05 mol % or less: R R R R Si Si R O O R P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, a silylphosphine compound rep-resented by the Formula (1) with a content of a compound represented by the following Formula (6) of 0.05 mol % or less: R R R R Si R O Si R O O P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by Formula (1) with a content of a compound represented by the following Formula (7) of 0.2 mol % or less: R R R Si R R Si P P Si R R Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein at least one selected from the group consisting of indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate and indium oleate is used as the ndium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein an indium carboxylate with no absorption peak derived from a hydroxyl group observed in the range of 1500 cm⁻¹ or more and 1700 cm⁻¹ or less in IR spectrum is used as the indium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a reaction between the phosphorus source and the indium source is performed at a temperature in the range of 20° C. or more and 150° C. or less.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in an organic solvent.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in the presence of a trialkylphosphine.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained by the method according to claim 1 to a temperature of 200° C. or more and 350° C. or less to obtain an InP quantum dot.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained B₂ by the method according to claim 1 together with a com-pound containing an element source M (M is at least one selected from the group consisting of Be, Mg, Ca, Mn, Cu, Zn, Cd, B, Al, Ga, N, As, Sb and Bi) other than a phospho-rous source and an indium source to a temperature of 200° C. or more and 350° C. or less to obtain a composite quantum dot of In, P and M.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Production of tris(trimethylsilyl)phosphine (TMSP) as the silylphosphine compound represented by Formula (1). Degassed/dehydrated toluene (189.8 kg), triethylamine (82 kg), trimethylsilyl trifluoromethanesulfonate (149.5 kg) were combined in a reaction vessel under nitrogen, liquid temperature adjusted to 30°C, then 7.4 kg of phosphine gas was fed over 3 hours. After aging at 35°C for 4 hours, the two-layer reaction solution was separated, concentrated under reduced pressure (6.3 kPa, 70°C), and distilled (0.5 kPa, 85°C column top). 49.3 kg of main fraction (TMSP) was collected. Purity and impurity content (Formulas (2)–(7)) were measured by 31P-NMR and GC. Results: TMSP 99.6 mol%, Formula (2) 0.15 mol%, Formula (3) N.D., Formula (4) 0.08 mol%, Formula (5) N.D.
2 materials1 process step
Production of tris(trimethylsilyl)phosphine using diethyl ether as solvent (156.9 g), triethylamine (82 g), trimethylsilyl trifluoromethanesulfonate (149.5 g), and 7.4 g phosphine gas. Similar process to Production Example 1 but with different solvent. Results: TMSP 98.3 mol%, Formula (2) 0.35 mol%, Formula (3) N.D., Formula (4) 0.18 mol%, Formula (5) 0.10 mol%.
2 materials1 process step
Production of indium myristate. Degraded indium acetate was used as a model hydroxyl group-containing indium carboxylate (commercially available indium acetate stored for ~100 days). Analysis by ICP emission spectrometer was performed.
Materials described outside the worked examples.
compound of Formula (2) — mono-H silylphosphine impurity
compound of Formula (3) — H₂P-SiR₃ impurity
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
TMSP purity — Production Example 1 | 99.6 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Production Example 1 |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
Cited non-patent literature · 3
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Patent
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US 11,692,134 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for producing an InP quantum dot precursor from a phosphorus source and an indium source, wherein a silylphosphine compound represented by the following For-mula (1) with a content of a compound represented by the following Formula (2) of 0.3 mol % or less: R R Si R R R P R Si Si R R R wherein each R is independently an alkyl group having 1 or more and 5 or less carbon atoms or an aryl group having 6 or more and 10 or less carbon atoms, H R R P R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (3) of 0.1 50 mol % or less: PH₂ Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (4) of 0.5 mol % or less: B₂ R R O R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (5) of 0.05 mol % or less: R R R R Si Si R O O R P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, a silylphosphine compound rep-resented by the Formula (1) with a content of a compound represented by the following Formula (6) of 0.05 mol % or less: R R R R Si R O Si R O O P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by Formula (1) with a content of a compound represented by the following Formula (7) of 0.2 mol % or less: R R R Si R R Si P P Si R R Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein at least one selected from the group consisting of indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate and indium oleate is used as the ndium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein an indium carboxylate with no absorption peak derived from a hydroxyl group observed in the range of 1500 cm⁻¹ or more and 1700 cm⁻¹ or less in IR spectrum is used as the indium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a reaction between the phosphorus source and the indium source is performed at a temperature in the range of 20° C. or more and 150° C. or less.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in an organic solvent.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in the presence of a trialkylphosphine.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained by the method according to claim 1 to a temperature of 200° C. or more and 350° C. or less to obtain an InP quantum dot.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained B₂ by the method according to claim 1 together with a com-pound containing an element source M (M is at least one selected from the group consisting of Be, Mg, Ca, Mn, Cu, Zn, Cd, B, Al, Ga, N, As, Sb and Bi) other than a phospho-rous source and an indium source to a temperature of 200° C. or more and 350° C. or less to obtain a composite quantum dot of In, P and M.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Production of tris(trimethylsilyl)phosphine (TMSP) as the silylphosphine compound represented by Formula (1). Degassed/dehydrated toluene (189.8 kg), triethylamine (82 kg), trimethylsilyl trifluoromethanesulfonate (149.5 kg) were combined in a reaction vessel under nitrogen, liquid temperature adjusted to 30°C, then 7.4 kg of phosphine gas was fed over 3 hours. After aging at 35°C for 4 hours, the two-layer reaction solution was separated, concentrated under reduced pressure (6.3 kPa, 70°C), and distilled (0.5 kPa, 85°C column top). 49.3 kg of main fraction (TMSP) was collected. Purity and impurity content (Formulas (2)–(7)) were measured by 31P-NMR and GC. Results: TMSP 99.6 mol%, Formula (2) 0.15 mol%, Formula (3) N.D., Formula (4) 0.08 mol%, Formula (5) N.D.
2 materials1 process step
Production of tris(trimethylsilyl)phosphine using diethyl ether as solvent (156.9 g), triethylamine (82 g), trimethylsilyl trifluoromethanesulfonate (149.5 g), and 7.4 g phosphine gas. Similar process to Production Example 1 but with different solvent. Results: TMSP 98.3 mol%, Formula (2) 0.35 mol%, Formula (3) N.D., Formula (4) 0.18 mol%, Formula (5) 0.10 mol%.
2 materials1 process step
Production of indium myristate. Degraded indium acetate was used as a model hydroxyl group-containing indium carboxylate (commercially available indium acetate stored for ~100 days). Analysis by ICP emission spectrometer was performed.
Materials described outside the worked examples.
compound of Formula (2) — mono-H silylphosphine impurity
compound of Formula (3) — H₂P-SiR₃ impurity
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
TMSP purity — Production Example 1 | 99.6 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Production Example 1 |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
Cited non-patent literature · 3
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Patent
Atlas literature
Patent
US 11,692,134 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for producing an InP quantum dot precursor from a phosphorus source and an indium source, wherein a silylphosphine compound represented by the following For-mula (1) with a content of a compound represented by the following Formula (2) of 0.3 mol % or less: R R Si R R R P R Si Si R R R wherein each R is independently an alkyl group having 1 or more and 5 or less carbon atoms or an aryl group having 6 or more and 10 or less carbon atoms, H R R P R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (3) of 0.1 50 mol % or less: PH₂ Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (4) of 0.5 mol % or less: B₂ R R O R Si Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by the Formula (1) with a content of a compound represented by the following Formula (5) of 0.05 mol % or less: R R R R Si Si R O O R P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, a silylphosphine compound rep-resented by the Formula (1) with a content of a compound represented by the following Formula (6) of 0.05 mol % or less: R R R R Si R O Si R O O P O Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a silylphosphine com-pound represented by Formula (1) with a content of a compound represented by the following Formula (7) of 0.2 mol % or less: R R R Si R R Si P P Si R R Si R R R wherein R is the same as in Formula (1) is used as the phosphorus source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein at least one selected from the group consisting of indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate and indium oleate is used as the ndium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein an indium carboxylate with no absorption peak derived from a hydroxyl group observed in the range of 1500 cm⁻¹ or more and 1700 cm⁻¹ or less in IR spectrum is used as the indium source.
The method for producing an InP quantum dot precur-sor according to claim 1, wherein a reaction between the phosphorus source and the indium source is performed at a temperature in the range of 20° C. or more and 150° C. or less.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in an organic solvent.
The method for producing an InP quantum dot precursor according to claim 1, wherein the reaction between the phosphorus source and the indium source is performed in the presence of a trialkylphosphine.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained by the method according to claim 1 to a temperature of 200° C. or more and 350° C. or less to obtain an InP quantum dot.
A method for producing an InP-based quantum dot comprising heating an InP quantum dot precursor obtained B₂ by the method according to claim 1 together with a com-pound containing an element source M (M is at least one selected from the group consisting of Be, Mg, Ca, Mn, Cu, Zn, Cd, B, Al, Ga, N, As, Sb and Bi) other than a phospho-rous source and an indium source to a temperature of 200° C. or more and 350° C. or less to obtain a composite quantum dot of In, P and M.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Production of tris(trimethylsilyl)phosphine (TMSP) as the silylphosphine compound represented by Formula (1). Degassed/dehydrated toluene (189.8 kg), triethylamine (82 kg), trimethylsilyl trifluoromethanesulfonate (149.5 kg) were combined in a reaction vessel under nitrogen, liquid temperature adjusted to 30°C, then 7.4 kg of phosphine gas was fed over 3 hours. After aging at 35°C for 4 hours, the two-layer reaction solution was separated, concentrated under reduced pressure (6.3 kPa, 70°C), and distilled (0.5 kPa, 85°C column top). 49.3 kg of main fraction (TMSP) was collected. Purity and impurity content (Formulas (2)–(7)) were measured by 31P-NMR and GC. Results: TMSP 99.6 mol%, Formula (2) 0.15 mol%, Formula (3) N.D., Formula (4) 0.08 mol%, Formula (5) N.D.
2 materials1 process step
Production of tris(trimethylsilyl)phosphine using diethyl ether as solvent (156.9 g), triethylamine (82 g), trimethylsilyl trifluoromethanesulfonate (149.5 g), and 7.4 g phosphine gas. Similar process to Production Example 1 but with different solvent. Results: TMSP 98.3 mol%, Formula (2) 0.35 mol%, Formula (3) N.D., Formula (4) 0.18 mol%, Formula (5) 0.10 mol%.
2 materials1 process step
Production of indium myristate. Degraded indium acetate was used as a model hydroxyl group-containing indium carboxylate (commercially available indium acetate stored for ~100 days). Analysis by ICP emission spectrometer was performed.
Materials described outside the worked examples.
compound of Formula (2) — mono-H silylphosphine impurity
compound of Formula (3) — H₂P-SiR₃ impurity
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 (b) is an IR spectrum of indium acetate that is a product of a first step 15 in Production Example 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
TMSP purity — Production Example 1 | 99.6 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Production Example 1 |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
Cited non-patent literature · 3
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compound of Formula (4) — disiloxane impurity
compound of Formula (5) — phosphonate-type siloxy impurity
compound of Formula (6) — phosphite-type siloxy impurity
compound of Formula (7) — diphosphinosilyl impurity
indium carboxylate (indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate, or indium oleate)
indium carboxylate with no hydroxyl absorption in 1500–1700 cm⁻¹ IR range
InP quantum dot
InP
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
| 0.15 mol% |
compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Production Example 1 | 0.08 mol% | compound of Formula (4) — disiloxane impurity |
TMSP purity — Comparative Production Example 1 | 98.3 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Comparative Production Example 1 | 0.35 mol% | compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Comparative Production Example 1 | 0.18 mol% | compound of Formula (4) — disiloxane impurity |
Formula (5) impurity in TMSP — Comparative Production Example 1 | 0.1 mol% | compound of Formula (5) — phosphonate-type siloxy impurity |
compound of Formula (4) — disiloxane impurity
compound of Formula (5) — phosphonate-type siloxy impurity
compound of Formula (6) — phosphite-type siloxy impurity
compound of Formula (7) — diphosphinosilyl impurity
indium carboxylate (indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate, or indium oleate)
indium carboxylate with no hydroxyl absorption in 1500–1700 cm⁻¹ IR range
InP quantum dot
InP
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
| 0.15 mol% |
compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Production Example 1 | 0.08 mol% | compound of Formula (4) — disiloxane impurity |
TMSP purity — Comparative Production Example 1 | 98.3 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Comparative Production Example 1 | 0.35 mol% | compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Comparative Production Example 1 | 0.18 mol% | compound of Formula (4) — disiloxane impurity |
Formula (5) impurity in TMSP — Comparative Production Example 1 | 0.1 mol% | compound of Formula (5) — phosphonate-type siloxy impurity |
compound of Formula (4) — disiloxane impurity
compound of Formula (5) — phosphonate-type siloxy impurity
compound of Formula (6) — phosphite-type siloxy impurity
compound of Formula (7) — diphosphinosilyl impurity
indium carboxylate (indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate, or indium oleate)
indium carboxylate with no hydroxyl absorption in 1500–1700 cm⁻¹ IR range
InP quantum dot
InP
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
| 0.15 mol% |
compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Production Example 1 | 0.08 mol% | compound of Formula (4) — disiloxane impurity |
TMSP purity — Comparative Production Example 1 | 98.3 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Comparative Production Example 1 | 0.35 mol% | compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Comparative Production Example 1 | 0.18 mol% | compound of Formula (4) — disiloxane impurity |
Formula (5) impurity in TMSP — Comparative Production Example 1 | 0.1 mol% | compound of Formula (5) — phosphonate-type siloxy impurity |
compound of Formula (4) — disiloxane impurity
compound of Formula (5) — phosphonate-type siloxy impurity
compound of Formula (6) — phosphite-type siloxy impurity
compound of Formula (7) — diphosphinosilyl impurity
indium carboxylate (indium acetate, indium laurate, indium myristate, indium palmitate, indium stearate, or indium oleate)
indium carboxylate with no hydroxyl absorption in 1500–1700 cm⁻¹ IR range
InP quantum dot
InP
FIG. 2 is an IR spectrum of indium myristate that is a product of a second step in Production Example 2.
FIG. 3 is an IR spectrum of indium myristate that is a product in Production Example 3. 20
FIG. 4 is a UV-VIS spectrum of a liquid containing the InP quantum dot precursor obtained in Example 1.
FIG. 5 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 1.
FIG. 6 is a UV-VIS spectrum of a liquid containing the 25 InP quantum dot precursor obtained in Example 3.
FIG. 7 is a UV-VIS spectrum of a liquid containing the InP quantum dot obtained in Example 3. DESCRIPTION OF EMBODIMENT 30 Hereinafter, preferred embodiments …
| 0.15 mol% |
compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Production Example 1 | 0.08 mol% | compound of Formula (4) — disiloxane impurity |
TMSP purity — Comparative Production Example 1 | 98.3 mol% | P(Si(CH₃)3)3 |
Formula (2) impurity in TMSP — Comparative Production Example 1 | 0.35 mol% | compound of Formula (2) — mono-H silylphosphine impurity |
Formula (4) impurity in TMSP — Comparative Production Example 1 | 0.18 mol% | compound of Formula (4) — disiloxane impurity |
Formula (5) impurity in TMSP — Comparative Production Example 1 | 0.1 mol% | compound of Formula (5) — phosphonate-type siloxy impurity |
