JP2011051821A - Method for producing compound semiconductor fine particle - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a compound semiconductor fine particle whose particle diameter distribution does not spread and capable of producing a compound semiconductor fine particle having a desired particle diameter. <P>SOLUTION: The method for producing a compound semiconductor fine particles includes a nucleation reaction step S21, a cooling step S22 and a nuclear growth reaction step S23. The nucleation reaction step forms a nucleus by reacting a plurality of solutions in which a raw material containing elements which compose a compound semiconductor and an organic compound are dissolved in a solvent and passing through a first capillary maintained at a first temperature at a first flow rate, and the cooling step cools the temperature of the solution containing the nucleus formed by the nucleation reaction step from the first temperature to a second temperature which is higher than the temperature wherein the organic compound deposits from the solution and lower than the temperature wherein the nucleus grows. The nuclear growth reaction step grows up the nucleus to a compound semiconductor fine particle by passing the solution which is cooled to the second temperature by the cooling step through a second capillary maintained at a third temperature at a second flow rate. <P>COPYRIGHT: (C)2011,JPO&amp;INPIT

Description

  The present invention relates to a method for producing compound semiconductor fine particles, and in particular, relates to a method for producing compound semiconductor fine particles by reacting a plurality of solutions in which a raw material containing an element constituting a compound semiconductor is dissolved in a solvent and circulating the solution through a capillary tube. .

  Compound semiconductor fine particles are materials having characteristics such as different wavelengths of light to be absorbed and different wavelengths of light to be emitted depending on the particle size. Already, compound semiconductor fine particles can be widely used as light emitting materials such as displays and light emitting diodes. In addition, since compound semiconductor fine particles have a feature that the half-value width of the wavelength of the emission band is narrow, it can be used as a marker for fluorescent immunoassay and a luminescent biological analysis reagent, such as a pigment. It can also be used as a coloring material.

  Patent Documents 1 and 2 disclose a method for producing compound semiconductor fine particles. In the method for producing compound semiconductor fine particles disclosed in Patent Document 1, a raw material containing an element belonging to Groups 11 to 13 of the periodic table and a raw material containing an element belonging to Groups 15 to 17 of the periodic table are independently provided. Thus, a method of producing compound semiconductor fine particles by flowing in a flow reactor equipped with a thin tube is disclosed.

  In the method for producing compound semiconductor fine particles disclosed in Patent Document 2, there is a method for producing compound semiconductor fine particles by performing stepwise a reaction for forming nuclei of compound semiconductor fine particles and a reaction for growing nuclei into compound semiconductor fine particles. It is disclosed. A continuous reaction apparatus is used for the reaction for forming the nuclei of the compound semiconductor fine particles, and a batch reaction apparatus is used for the reaction for growing the nuclei into the compound semiconductor fine particles.

JP 2003-160336 A JP 2007-224233 A

  However, the compound semiconductor fine particle manufacturing method disclosed in Patent Document 1 is manufactured because a reaction for forming nuclei of compound semiconductor fine particles and a reaction for growing nuclei are performed together in a flow reactor. The compound semiconductor fine particles have a mixture of compound semiconductor fine particles and compound semiconductor fine particles grown from the nuclei, resulting in a problem that the particle size distribution of the compound semiconductor fine particles cannot be narrowed.

  In addition, in the method for producing compound semiconductor fine particles disclosed in Patent Document 2, since the reaction for forming the nuclei of the compound semiconductor fine particles and the reaction for growing the nuclei are performed in stages, the nuclei of the compound semiconductor fine particles, There is no possibility of mixing with compound semiconductor fine particles grown from the above. However, since the reaction for growing the nuclei is performed in a batch reactor, there is a problem that the particle size distribution of the compound semiconductor fine particles cannot be narrowed if temperature unevenness occurs in the batch reactor.

  The present invention has been made in view of the above circumstances, and provides a method for producing compound semiconductor fine particles capable of producing compound semiconductor fine particles having a desired particle size with a narrow particle size distribution of the compound semiconductor fine particles. With the goal.

  In order to achieve the above object, a method for producing compound semiconductor fine particles according to the first invention comprises reacting a plurality of solutions in which a raw material containing at least an element constituting a compound semiconductor and an organic compound are dissolved in a solvent, to thereby obtain a first temperature. A nucleation reaction step for forming nuclei by flowing at a first flow rate through a first capillary tube maintained at a temperature, and a temperature of a solution containing the nuclei formed in the nucleation reaction step from the first temperature, the organic compound Cooling to a second temperature higher than the temperature at which the solution precipitates from the solution and lower than the temperature at which the nuclei grow, and the solution cooled to the second temperature in the cooling step into the second capillary tube maintained at the third temperature A nuclear growth reaction step of growing nuclei into compound semiconductor fine particles by flowing at a second flow rate.

  Further, the method for producing compound semiconductor fine particles according to the second invention includes a storage step of storing the solution cooled to the second temperature in the cooling step in a container kept at the second temperature in the first invention, In the nucleus growth reaction step, the solution stored in the vessel cooled at the cooling step and kept at the second temperature is circulated through the second capillary.

  In the method for producing compound semiconductor fine particles according to the third invention, in the first or second invention, the nucleus growth reaction step is repeated using the solution circulated through the second capillary in the nucleus growth reaction step.

  In the method for producing compound semiconductor fine particles according to the fourth invention, in any one of the first to third inventions, a tube cross-sectional area and / or a tube length of the second capillary is different from that of the first capillary.

  In the first aspect of the invention, the solution containing the nuclei formed by circulating the first tubule at the first temperature at the first flow rate is cooled from the first temperature to the second temperature. The growth is stopped and the nuclei of the compound semiconductor fine particles and the compound semiconductor fine particles grown from the nuclei are not mixed. Further, since the compound semiconductor fine particles are grown by allowing the solution containing the nucleus cooled to the second temperature to flow through the second capillary maintained at the third temperature at the second flow rate to grow the compound semiconductor fine particles, the solution is formed in the second capillary for growing the nucleus. Compound semiconductor fine particles having a narrow particle size distribution without temperature unevenness can be produced.

  In the second invention, since the cooled solution is stored in a container kept at the second temperature, even when the second flow rate of the second capillary is slower than the first flow rate of the first capillary, the compound semiconductor nucleus grows. The nuclear growth reaction step can be sequentially performed without causing the organic compound to precipitate from the solution, and the compound semiconductor fine particles having a narrow particle size distribution can be produced.

  In the third invention, compound semiconductor fine particles having a desired particle diameter can be produced by repeatedly performing the nucleus growth reaction step using the solution circulated in the second capillary tube in the nucleus growth reaction step.

  In the fourth invention, the first capillary and the second capillary have different tube cross-sectional areas and / or tube lengths, so that the size of the compound semiconductor particles growing from the nucleus is controlled to produce compound semiconductor particles having a desired particle size. can do.

  In the method for producing compound semiconductor fine particles according to the present invention, a plurality of solutions in which a raw material containing an element constituting a compound semiconductor is dissolved in a solvent are reacted, and distributed at a first flow rate through a first capillary maintained at a first temperature. The temperature of the nucleation reaction step for forming nuclei and the temperature of the solution containing the nuclei formed in the nucleation reaction step is higher from the first temperature than the temperature at which the organic compound is precipitated from the solution and lower than the temperature at which the nuclei grow. Cooling step for cooling to the second temperature, and nucleus growth for growing nuclei into compound semiconductor fine particles by circulating the solution cooled to the second temperature in the cooling step through the second capillary maintained at the third temperature at the second flow rate Since the reaction step is included, the compound semiconductor fine particles having a narrow particle size distribution can be manufactured without mixing the nuclei of the compound semiconductor fine particles and the compound semiconductor fine particles grown from the nuclei.

It is a schematic diagram which shows the structure of the manufacturing apparatus used for the manufacturing method of the compound semiconductor fine particle concerning embodiment of this invention. It is a flowchart for demonstrating the manufacturing method of the compound semiconductor fine particle concerning embodiment of this invention. It is an illustration figure of the TEM photograph of the compound semiconductor fine particle of CdSe manufactured with the manufacturing method of the compound semiconductor fine particle concerning embodiment of this invention. It is an illustration figure of another TEM photograph of the compound semiconductor fine particle of CdSe manufactured with the manufacturing method of the compound semiconductor fine particle concerning embodiment of this invention. It is an illustration figure of the photoluminescence spectrum of the compound semiconductor fine particle of CdSe manufactured with the manufacturing method of the compound semiconductor fine particle concerning embodiment of this invention. It is an illustration figure of the photoluminescence spectrum of the compound semiconductor fine particle of CdSe manufactured with another manufacturing method as a comparative example.

  Hereinafter, a method for producing compound semiconductor fine particles in an embodiment of the present invention will be specifically described with reference to the drawings. The following embodiments do not limit the invention described in the claims, and all combinations of characteristic items described in the embodiments are essential to the solution. It goes without saying that it is not limited.

  The method for producing compound semiconductor fine particles according to the embodiment of the present invention is a method for growing a compound semiconductor crystal by injecting a thermally decomposable compound semiconductor raw material into a high-temperature coordination organic compound. FIG. 1 is a schematic diagram showing the configuration of a manufacturing apparatus used in the method for manufacturing compound semiconductor fine particles according to the embodiment of the present invention. As shown in FIG. 1, a compound semiconductor fine particle manufacturing apparatus A includes a raw material containing an element (for example, Cd) constituting a compound semiconductor (for example, CdSe), an organic compound (for example, stearic acid (surfactant), A container 1 of a first solution in which octylphosphine oxide, octadecylamine, and the like are dissolved in a solvent, a raw material containing an element (for example, Se) constituting a compound semiconductor, and an organic compound (for example, stearic acid (surfactant)), A second solution container 2 in which trioctylphosphine oxide, octadecylamine, etc.) are dissolved in a solvent, and a third solution obtained by reacting the first solution and the second solution is circulated through the narrow tube (first narrow tube). And a nucleation reactor 3 for forming nuclei of compound semiconductor fine particles. Furthermore, the compound semiconductor fine particle manufacturing apparatus A allows the third solution containing the nuclei formed in the nucleation reactor 3 to be collected and stored, and the third solution containing the nuclei to flow through the narrow tube (second thin tube). Thus, a nuclear growth reactor 5 for growing nuclei into compound semiconductor fine particles and a container 6 for collecting the third solution containing the compound semiconductor fine particles formed in the nuclear growth reactor 5 are provided. In the first solution and the second solution, the organic compound is added to the raw material containing the element constituting the compound semiconductor because the dissolution and stabilization of the raw material containing the element constituting the compound semiconductor in the solution in the solvent This is to improve the dispersion stability by coordination with the compound semiconductor fine particles.

The container 1 includes a temperature controller 11 for adjusting the temperature of the first solution, the container 2 includes a temperature controller 21 for adjusting the temperature of the second solution, and the container 4 includes a nucleus. A temperature controller 41 for adjusting the temperature of the third solution is provided, and the container 6 is provided with a temperature controller 61 for adjusting the temperature of the third solution containing the compound semiconductor fine particles. Further, the nucleation reactor 3 has a narrow tube (first thin tube) that allows the third solution to flow at a predetermined flow rate, and a temperature controller 31 that adjusts the temperature of the third solution that flows through the narrow tube. The nuclear growth reactor 5 includes a narrow tube (second thin tube) that allows the third solution containing the nucleus to flow at a predetermined flow rate, and a temperature controller for adjusting the temperature of the third solution that includes the nucleus that flows through the narrow tube. 51. Note that the tubules of the nucleation reactor 3 and the nucleation growth reactor 5 have, for example, a tube cross-sectional area of 0.0009 cm ² and a tube length of 120 cm. Have. However, the tube cross-sectional area and / or tube length of the thin tube (second thin tube) of the nuclear growth reactor 5 is limited to the case where the tube cross-sectional area and / or tube length of the thin tube (first thin tube) of the nucleation reactor 3 is the same. The tubule of the nucleation reactor 3 (first tubule) and the tubule of the nucleus growth reactor 5 (second tubule) are tubes so that the compound semiconductor fine particles grown from the nucleus have a desired particle size. The cross-sectional area and / or the tube length may be different.

  Between the container 1 and the nucleation reactor 3, a liquid feed pump 13 for supplying the first solution from the container 1 to the nucleation reactor 3 is provided between the container 2 and the nucleation reactor 3. A liquid feed pump 23 for supplying the second solution from the container 2 to the nucleation reactor 3 is provided. Further, a liquid feed pump 45 for supplying a third solution containing nuclei from the container 4 to the nucleus growth reactor 5 is provided between the container 4 and the nucleus growth reactor 5. Furthermore, a temperature controller 34 is provided between the nucleation reactor 3 and the container 4 for adjusting the temperature of the third solution containing the nuclei collected and stored in the container 4 and the temperature of the container 4.

  Next, a method for producing CdSe compound semiconductor fine particles using the compound semiconductor fine particle production apparatus A will be described. FIG. 2 is a flowchart for explaining the method for producing compound semiconductor fine particles according to the embodiment of the present invention. As shown in FIG. 2, first, in the nucleation reaction step S21, a first solution in which a raw material containing a Cd element and an organic compound constituting a compound semiconductor of CdSe are dissolved in a solvent, a raw material containing an Se element, and an organic compound The CdSe compound semiconductor is made to flow at a first flow rate through the third tube (first tube) of the nucleation reactor 3 maintained at the first temperature with the third solution obtained by reacting the second solution in which the solution is dissolved in a solvent. Form nuclei of fine particles. Specifically, 1 g of cadmium oxide (CdO), 160 g of octadecene (solvent), 10 g of stearic acid (surfactant), 20 g of trioctylphosphine oxide, and 60 g of octadecylamine are put into the container 1, and 30 minutes at 100 ° C. under reduced pressure. The first solution produced by the deaeration process is heated to 280 ° C. (first temperature) using the temperature controller 11.

  6 g of selenium, 110 g of octadecene (solvent), and 20 g of tributylphosphine are put into the container 2, heated to 100 ° C. in a nitrogen atmosphere and dissolved in octelecene for about 2 hours, and the second solution produced is controlled in temperature. Cool to room temperature (25 ° C.) using vessel 21.

  The first solution in the container 1 is supplied to the nucleation reactor 3 at a flow rate of 6.7 ml / s using the liquid feed pump 13, and the second solution in the container 2 is supplied to the nucleation reactor 3 using the liquid feed pump 23. Feed to nucleation reactor 3 at a flow rate of 4 ml / s. The third solution obtained by reacting the first solution and the second solution supplied to the nucleation reactor 3 in the tubule (first tubule) of the nucleation reactor 3 is passed through the tubule at a predetermined flow rate (first flow rate). Circulate. The third solution heated to 280 ° C. (first temperature) using the temperature controller 31 is passed through the tubule of the nucleation reactor 3 at a predetermined flow rate so that the compound semiconductor fine particles of CdSe are contained in the third solution. Nuclei are formed. The predetermined flow rate (first flow rate) includes a flow rate for supplying the first solution to the nucleation reactor 3 (6.7 ml / s) and a flow rate for supplying the second solution to the nucleation reactor 3 (3.4 ml). / S). Moreover, the ratio with which the 1st solution and the 2nd solution are made to react can be adjusted by adjusting the flow rate of a 1st solution and the flow rate of a 2nd solution.

  Next, in the cooling step S22, the temperature of the third solution containing the nuclei formed in the nucleation reaction step S21 is changed from 280 ° C. (first temperature) to an organic compound (for example, stearic acid (surfactant), trioctyl). Phosphine oxide, octadecylamine, etc.) are cooled to 60 ° C. (second temperature), which is higher than the temperature at which the third solution precipitates and lower than the temperature at which the nuclei grow. Specifically, when the third solution containing nuclei formed in the nucleation reactor 3 is supplied from the nucleation reactor 3 to the container 4, the third solution is cooled to 60 ° C. using the temperature controller 34. By cooling the third solution containing the nuclei to 60 ° C., the growth of the nuclei is stopped. The temperature at which the third solution containing nuclei is cooled is not limited to 60 ° C., as long as the temperature is higher than the temperature at which the organic compound precipitates from the third solution and lower than the temperature at which the nuclei grow. Any temperature is acceptable. The third solution containing the nucleus is cooled to 60 ° C. using the temperature controller 34, and then is collected and stored in the container 4 filled with nitrogen and kept at 60 ° C. (second temperature).

  Next, in the nucleus growth reaction step S23, the third solution containing the nucleus cooled to 60 ° C. (second temperature) collected and stored in the container 4 in the cooling step S22 is maintained at 250 ° C. (third temperature). The nucleus is grown into CdSe compound semiconductor fine particles by flowing through the thin tube (second thin tube) of the growth reactor 5 at 0.2 ml / s (second flow rate). Specifically, the third solution containing the nuclei collected and stored in the container 4 is supplied to the nucleation growth reactor 5 at a flow rate of 0.2 ml / s using the liquid feed pump 45. The third solution containing the nuclei heated to 250 ° C. using the temperature controller 51 is circulated through the thin tube of the nuclear growth reactor 5 at a flow rate of 0.2 ml / s, so that the nuclei contained in the third solution. Grow into compound semiconductor fine particles having a desired particle size. The third solution containing compound semiconductor fine particles supplied from the nuclear growth reactor 5 is collected in the container 6.

  Here, the third solution containing the nuclei cooled by using the temperature controller 34 is temporarily collected and stored in the container 4 without directly supplying the nucleation growth reactor 5, so that the third solution containing the nuclei is obtained. The third solution containing nuclei is transferred to the tubule of the nucleation reactor 5 at a lower flow rate than the flow rate circulated to the tubule of the nucleation reactor 3 without affecting the flow rate of the nucleation reactor 3. It can be distributed. That is, the container 4 functions as a buffer for adjusting the third solution containing the nuclei supplied from the nucleation reactor 3 so that the third solution can be sequentially passed through the tubules of the nucleation growth reactor 5. It should be noted that there is no difference between the flow rate flowing through the tubule of the nucleation reactor 3 and the flow rate flowing through the tubule of the nucleus growth reactor 5, or the third including the nuclei supplied from the nucleation reactor 3. When the solution is circulated through the thin tubes of the plurality of nuclear growth reactors 5, it is not necessary to provide the container 4.

  In the method for producing compound semiconductor fine particles according to the embodiment of the present invention, the third solution containing nuclei is not only passed through the capillary tube of the nuclear growth reactor 5 but once grown into compound semiconductor fine particles having a desired particle size. For this purpose, the third solution containing the compound semiconductor fine particles recovered in the container 6 is repeatedly circulated through the narrow tube of the nuclear growth reactor 5. That is, the third solution containing the compound semiconductor fine particles recovered in the container 6 is returned to the container 4, and 0.2 ml of the third solution heated to 250 ° C. using the temperature controller 51 is placed in the thin tube of the nuclear growth reactor 5. By flowing again at a flow rate of / s, the compound semiconductor fine particles contained in the third solution are grown so as to have a desired particle size. In addition, the 3rd solution which distribute | circulated the thin tube of the nuclear growth reactor 5 again is collect | recovered with the container 6, and the 3rd solution collect | recovered in the container 6 is diluted with 240 ml of toluene.

  In order to observe the CdSe compound semiconductor fine particles taken out from the diluted third solution, a TEM (transmission electron microscope) is used. In order to observe the CdSe compound semiconductor fine particles with TEM, it is necessary to drop the diluted third solution onto a Cu mesh with a carbon film for TEM and dry it. FIG. 3 is an exemplary TEM photograph of CdSe compound semiconductor fine particles produced by the method for producing compound semiconductor fine particles according to the embodiment of the present invention. FIG. 4 is another exemplary view of a TEM photograph of CdSe compound semiconductor fine particles produced by the method for producing compound semiconductor fine particles according to the embodiment of the present invention. FIG. 3 shows CdSe compound semiconductor fine particles magnified 59,000 times, and each of the CdSe compound semiconductor fine particles appearing as black granules is a CdSe compound semiconductor fine particle. FIG. 4 shows CdSe compound semiconductor fine particles magnified 590,000 times, and a circle indicates one CdSe compound semiconductor fine particle. From the TEM photograph, it can be seen that the compound semiconductor fine particles of CdSe produced by the method for producing compound semiconductor fine particles according to the embodiment of the present invention have almost the same particle size, and the particle size is about 4 nm.

  Next, in order to examine the particle size distribution of the CdSe compound semiconductor fine particles produced by the method for producing compound semiconductor fine particles according to the embodiment of the present invention, the photoluminescence spectrum of the diluted third solution is measured. For photoluminescence spectrum, the diluted third solution is set in the sample holder of the integrating sphere, and the sample holder is irradiated with UV light having a center wavelength of 300 nm (half-value width of 7 nm or less) obtained from the light source of the xenon lamp through the monochromator. It can be obtained by measuring light emitted from light with a CCD sensor. In addition, based on the measured photoluminescence spectrum, the number of photons of excitation light absorbed by the diluted third solution (number of absorbed light photons) and the number of photons of light emitted by the diluted third solution (number of emitted photons) The ratio was calculated as quantum efficiency (%) (= number of emitted photons / number of absorbed light photons × 100).

  FIG. 5 is an exemplary diagram of a photoluminescence spectrum of CdSe compound semiconductor fine particles produced by the method for producing compound semiconductor fine particles according to the embodiment of the present invention. In FIG. 5, the horizontal axis represents wavelength (nm) and the vertical axis represents photoluminescence intensity. The photoluminescence spectrum of the compound semiconductor fine particles of CdSe produced by the method for producing compound semiconductor fine particles according to the present embodiment has a wavelength difference at a photoluminescence intensity at which the peak wavelength is 598.01 nm and the photoluminescence intensity at the peak wavelength is halved. The full width at half maximum is 33.89 nm and the quantum efficiency is 48%.

  As a comparative example, the nuclei contained in the third solution in the container 4 without supplying the third solution containing the nuclei collected and stored in the container 4 to the nucleus growth reactor 5 using the liquid feed pump 45. Is grown to produce compound semiconductor fine particles, and the photoluminescence spectrum of the compound semiconductor fine particles is measured. Specifically, in order to grow nuclei contained in the third solution in the container 4, the container 4 is heated to 250 ° C. using the temperature controller 41, held for 1 hour, and then cooled to 60 ° C. The third solution is diluted with 240 ml of toluene. In addition, the manufacturing method of the compound semiconductor fine particle of the comparative example is similar to the manufacturing method of the compound semiconductor fine particle disclosed in Patent Document 2.

  FIG. 6 is an exemplary diagram of a photoluminescence spectrum of a CdSe compound semiconductor fine particle produced by another production method as a comparative example. As shown in FIG. 6, the photoluminescence spectrum of a CdSe compound semiconductor fine particle produced by another method for producing compound semiconductor fine particles as a comparative example has a peak wavelength of 597.27 nm, a half width of 63.92 nm, and a quantum efficiency of 30. %. As a comparative example, the photoluminescence spectrum of a compound semiconductor fine particle of CdSe produced by another production method is compared with the photoluminescence spectrum of a compound semiconductor fine particle of CdSe produced by the method of producing a compound semiconductor fine particle according to the embodiment of the present invention. It can be seen that the full width at half maximum is increased about 1.9 times. That is, the particle size distribution of the compound semiconductor fine particles of CdSe manufactured by the method of manufacturing compound semiconductor fine particles according to the embodiment of the present invention is larger than the particle size distribution of the compound semiconductor fine particles of CdSe manufactured by another manufacturing method as a comparative example. You can see that it is narrow.

  As described above, in the method for producing compound semiconductor fine particles according to the embodiment of the present invention, the third solution obtained by reacting the first solution and the second solution is placed in the first capillary tube maintained at the first temperature. Nuclei are formed by flowing at a flow rate, and the temperature of the third solution containing the nuclei is cooled from the first temperature to the second temperature, so that the compound semiconductor nuclei and the compound semiconductor fine particles grown from the nuclei coexist. There is nothing. Further, since the third solution cooled to the second temperature is allowed to flow at a second flow rate through the second capillary maintained at the third temperature at the second flow rate, the nucleus grows into the compound semiconductor fine particles. Compound semiconductor fine particles having a narrow particle size distribution without temperature unevenness in the third solution can be produced.

  The method for producing compound semiconductor particles according to the embodiment of the present invention is not limited to the production of CdSe compound semiconductor particles, but II (Group 12) -VI (Group 16) group compound semiconductor particles. (For example, ZnTe, ZnSe, ZnS, etc.), III (Group 13) -V (Group 15) group compound semiconductor fine particles (for example, InAs etc.) can be applied to the production of any compound semiconductor fine particles.

  Further, in the method for producing compound semiconductor fine particles according to the embodiment of the present invention, the method for producing compound semiconductor fine particles having a desired particle diameter is a method in which the third solution is circulated through the capillary of the nuclear growth reactor 5 a plurality of times. The method is not limited and may be a method in which the tube cross-sectional area and / or the tube length is changed once through the narrow tube of the nuclear growth reactor 5. The tube cross-sectional area and / or tube length of the thin tube of the nuclear growth reactor 5 is determined by the desired particle size of the compound semiconductor fine particles to be produced. It should be noted that a plurality of compound semiconductor fine particles having different desired particle diameters can be produced in the same step by providing a plurality of nuclear growth reactors 5 having thin tubes having different tube cross-sectional areas and / or tube lengths.

  Furthermore, the compound semiconductor fine particle manufacturing method according to the embodiment of the present invention is a compound semiconductor fine particle manufacturing apparatus A that includes the tubule of the nucleation reactor 3 and the thin tube of the nucleation growth reactor 5 independently. The method is not limited to the method for producing fine particles, and the compound semiconductor fine particles may be produced by a compound semiconductor fine particle production apparatus that uses the fine tube of the nucleation reactor 3 as the fine tube of the nuclear growth reactor 5. That is, in the compound semiconductor fine particle production apparatus A shown in FIG. 1, the third solution containing the nuclei collected and stored in the container 4 is circulated through the tubule of the nucleation reactor 3 at the second flow rate. It is also possible to produce compound semiconductor fine particles with a configuration in which the nuclear growth reactor 5 is not provided. The inexpensive method for producing compound semiconductor fine particles using the thin tube of the nucleation reactor 3 as the thin tube of the nuclear growth reactor 5 can also apply the method for producing the compound semiconductor fine particles according to the embodiment of the present invention.

1, 2, 4, 6 Container 3 Nucleation reactor 5 Nucleation growth reactor 11, 21, 31, 34, 41, 51, 61 Temperature controller 13, 23, 45 Liquid feed pump

Claims (4)

Nuclei that form nuclei by reacting a plurality of solutions in which a raw material containing an element constituting at least a compound semiconductor and an organic compound are dissolved in a solvent and circulating the solution through a first capillary maintained at a first temperature at a first flow rate. A formation reaction step;
A cooling step of cooling the temperature of the solution containing the nuclei formed in the nucleation reaction step from the first temperature to a second temperature higher than a temperature at which the organic compound precipitates from the solution and lower than a temperature at which the nuclei grow; ,
And a nucleus growth reaction step in which the solution cooled to the second temperature in the cooling step is passed through a second capillary maintained at the third temperature at a second flow rate to grow nuclei into compound semiconductor fine particles. A method for producing compound semiconductor fine particles. Storing the solution cooled to the second temperature in the cooling step in a container maintained at the second temperature;
2. The compound semiconductor fine particle according to claim 1, wherein in the nuclear growth reaction step, the solution stored in the container that is cooled in the cooling step and maintained at the second temperature is circulated through the second capillary tube. Manufacturing method.   3. The method for producing compound semiconductor fine particles according to claim 1, wherein the nuclear growth reaction step is repeated using the solution circulated through the second capillary in the nuclear growth reaction step.   4. The method for producing compound semiconductor fine particles according to claim 1, wherein a tube cross-sectional area and / or a tube length of the second capillary tube is different from that of the first capillary tube.

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