CN112374474B - Preparation method of compact ultrahigh-purity material - Google Patents
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Abstract
Compared with the existing red phosphorus/arsenic production and purification process, the whole conversion process is carried out in a closed quartz tube, the influence of the environment on the product is avoided, the temperature of a high-temperature region and a low-temperature region is accurately controlled, so that non-compact arsenic/phosphorus particles in the high-temperature region are transferred to the low-temperature region in a gaseous form, are subjected to sublimation, nucleation and growth to obtain compact arsenic or phosphorus, and high-boiling-point impurity elements are still left in the high-temperature region, so that the first-step purification of the arsenic/phosphorus is realized. And in the final stage of cooling, controlling the temperature of the compact arsenic or phosphorus area to be higher than that of other areas all the time, so that impurity elements such as Cl, S and the like with low boiling points are condensed at the other end, and realizing the second-step purification of arsenic/phosphorus.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a preparation method of a compact ultrahigh-purity material.
Background
Ultra-pure arsenic and red phosphorus (purity greater than 99.9999%) are the main raw materials for preparing compound semiconductors such as gallium arsenide and indium phosphide, and are also one of the main doping elements of single crystals such as silicon and germanium, and ultra-pure red phosphorus and arsenic (purity greater than 99.99999%) are also used in the Molecular Beam Epitaxy (MBE) doping of wafers. The main process for preparing high-purity red phosphorus and arsenic at present is to chlorinate raw yellow phosphorus or arsenic with chlorine to obtain arsenic and phosphorus chlorides, and then to remove impurities by rectification according to the difference of the boiling points of the chlorides and the chlorides of impurity elements. Then reducing the rectified and purified arsenic chloride or phosphorus chloride by hydrogen under micro-positive pressure to obtain corresponding simple substances, phosphorus and arsenic.
Arsenic does not have a melting point under normal pressure, so arsenic obtained by reducing arsenic chloride with hydrogen is usually sponge-like arsenic, surface gaps are more and are not dense, and excessive appearance defects usually contain a large amount of impurity elements to interfere product detection. Compared with arsenic, high-purity red phosphorus is usually obtained by converting high-purity yellow phosphorus which is heated to about a boiling point under normal pressure, the red phosphorus obtained by converting the normal pressure has low density and is easy to fall off powder, and a small amount of yellow phosphorus can be mixed in the red phosphorus.
Disclosure of Invention
The invention aims to provide a preparation method of a compact ultrahigh-purity material, wherein the arsenic and red phosphorus prepared by the preparation method disclosed by the invention are high in purity and compact, and can meet the requirements of single crystal growth doping of MBE, si, ge and the like.
The invention provides a preparation method of a compact ultrahigh-purity material, which comprises the following steps:
a) Placing the raw material in a first temperature zone of a quartz tube, heating, sublimating the raw material in a second temperature zone of the quartz tube, and obtaining an intermediate product;
in the heating process, the temperature of the first temperature zone is 50-100 ℃ higher than that of the second temperature zone;
b) Keeping the temperature difference of the first temperature zone 50-100 ℃ higher than that of the second temperature zone to carry out integral cooling, firstly cooling the temperature of the second temperature zone to be 30-50 ℃ lower than the sublimation temperature of the intermediate product under normal pressure, preserving heat for 2-4 hours, and then cooling to be 50-80 ℃ lower than the sublimation temperature of the intermediate product under normal pressure;
c) And stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone until the temperature of the first temperature zone is 100-120 ℃ lower than that of the second temperature zone, and finally synchronously reducing the temperatures of the first temperature zone and the second temperature zone to the normal temperature to obtain the compact ultrahigh-purity material.
Preferably, the raw material is arsenic or red phosphorus, and the purity of the raw material is 5N-7N.
Preferably, the quartz tube is arranged in the pressure container, and the external pressure of the quartz tube is greater than the internal pressure.
Preferably, the temperature of the first temperature zone heated in the step A) is 95-110% of the temperature corresponding to the triple point of the raw material; the heating time is 2-10 hours.
Preferably, the quartz tube is evacuated, and the pressure vessel is filled with a protective gas.
Preferably, the pressure P at the corresponding temperature T is calculated from the relationship between temperature and pressure in the Antoine equation lgP = a-B (T + C) for red phosphorus and arsenic, and then the pressure vessel is filled with a protective gas at a pressure of P +1 atm.
Preferably, when the raw material is arsenic, the raw material is heated in the step A) until the temperature of the first temperature zone is 750-900 ℃;
in the step B), the temperature of the first temperature zone is firstly reduced to 600-700 ℃, the temperature is preserved for 2-4 hours, and then the temperature is reduced to 500-600 ℃ of the first temperature zone;
stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone to 350-450 ℃, and finally synchronously reducing the temperature to the normal temperature.
Preferably, when the raw material is red phosphorus, the raw material is heated in the step A) until the temperature of the first temperature zone is 550-700 ℃;
in the step B), the temperature of the first temperature zone is firstly reduced to 400-500 ℃, the temperature is preserved for 2-4 hours, and then the temperature is reduced to 300-400 ℃ of the first temperature zone;
and stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone to 150-250 ℃, and finally synchronously reducing the temperature to the normal temperature.
The invention provides a preparation method of a compact ultrahigh-purity material, which comprises the following steps: a) Placing the raw material in a first temperature zone of a quartz tube, heating, sublimating the raw material in a second temperature zone of the quartz tube to obtain an intermediate product; in the heating process, the temperature of the first temperature zone is 50-100 ℃ higher than that of the second temperature zone; b) Keeping the temperature difference of the first temperature zone 50-100 ℃ higher than that of the second temperature zone to carry out integral cooling, firstly cooling the temperature of the second temperature zone to be 30-50 ℃ lower than the sublimation temperature of the intermediate product under normal pressure, preserving heat for 2-4 hours, and then cooling to be 50-80 ℃ lower than the sublimation temperature of the intermediate product under normal pressure; c) And stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone until the temperature of the first temperature zone is 100-120 ℃ lower than that of the second temperature zone, and finally synchronously reducing the temperatures of the first temperature zone and the second temperature zone to the normal temperature to obtain the compact ultrahigh-purity material. Compared with the existing red phosphorus/arsenic production and purification process, the whole conversion process is carried out in a closed quartz tube, the influence of the environment on the product is avoided, the temperature of the high-temperature and low-temperature regions is accurately controlled, so that the non-compact arsenic/phosphorus particles in the high-temperature region are transferred to the low-temperature region in a gaseous form, then are subjected to desublimation, nucleation and growth to obtain compact arsenic or phosphorus, and the high-boiling-point impurity elements are still left in the high-temperature region, so that the first-step purification of the arsenic/phosphorus is realized. And in the final stage of cooling, controlling the temperature of the compact arsenic or phosphorus area to be higher than that of other areas all the time, so that impurity elements such as Cl, S and the like with low boiling points are condensed at the other end, and realizing the second-step purification of arsenic/phosphorus.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural view of a compact ultra-high purity material preparation apparatus according to the present invention;
1 is a pressure container, 2 is a heater, 3 is a quartz tube, 4 is a first temperature zone, and 5 is a second temperature zone.
Detailed Description
The invention provides a preparation method of a compact ultrahigh-purity material, which comprises the following steps:
a) Placing the raw material in a first temperature zone of a quartz tube, heating, sublimating the raw material in a second temperature zone of the quartz tube to obtain an intermediate product;
in the heating process, the temperature of the first temperature zone is 50-100 ℃ higher than that of the second temperature zone;
b) Keeping the temperature difference of the first temperature zone 50-100 ℃ higher than that of the second temperature zone to carry out integral cooling, firstly cooling the temperature of the second temperature zone to be 30-50 ℃ lower than the sublimation temperature of the intermediate product under normal pressure, preserving heat for 2-4 hours, and then cooling to be 50-80 ℃ lower than the sublimation temperature of the intermediate product under normal pressure;
c) And stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone until the temperature of the first temperature zone is 100-120 ℃ lower than that of the second temperature zone, and finally synchronously reducing the temperatures of the first temperature zone and the second temperature zone to the normal temperature to obtain the compact ultrahigh-purity material.
In the present invention, the raw material for preparing the dense ultra-high purity material is preferably arsenic or red phosphorus, and the purity of the raw material is preferably 5N to 7N, and more preferably, may be 5.5N or 7N.
The preparation process is completed in a closed quartz tube, a heater is arranged outside the quartz tube and consists of two temperature zones, the two temperature zones can be independently heated, and the heater and the quartz tube are placed in a stainless steel pressure container together.
The raw materials are sealed in the quartz tube, and the quartz tube is vacuumized before sealing. And pouring the raw material red phosphorus/arsenic to one end of the quartz tube after sealing, slowly pushing the quartz tube into a horizontal heater, wherein the heater consists of two heating temperature zones, and ensures that the arsenic or phosphorus in the quartz tube is positioned in one temperature zone (named as a first temperature zone) in the heater, and the other heating zone is a second temperature zone. And then putting the heater and the sealed quartz tube into a stainless steel pressure container integrally.
Before heating, the temperatures of the two temperature zones of the heater and the time required for reaching the target temperature are respectively set, and the temperature of the first temperature zone is always kept higher than the temperature of the temperature zone without arsenic and phosphorus (named as a second temperature zone) by more than 50 ℃, preferably 50-100 ℃, and more preferably 50-80 ℃ in the whole temperature rising process.
Along with the rise of the internal temperature of the heater, the granular red phosphorus/arsenic is slowly sublimated to be changed into a gaseous state, the internal pressure of the quartz tube is gradually increased, and in order to avoid explosion of the quartz tube caused by overhigh internal pressure of the quartz tube, inert gas needs to be filled into the pressure container to balance the pressure difference between the inside and the outside of the quartz tube.
The pressure P at the corresponding temperature T needs to be calculated according to the relationship between temperature and pressure in the red phosphorus and arsenic Antoine equation lgP = a-B (T + C). And then filling inert gas with the pressure of P +1atm into the pressure container outside the quartz tube through the gas inlet hole to ensure that the pressure outside the quartz tube is higher than the internal pressure. Typically the temperature T at which the pressure is calculated should be selected based on the actual measured temperature of the zone in which the heater temperature is higher.
The difference of the temperatures of the two temperature zones of the heater causes the difference of the saturated vapor pressures of phosphorus and arsenic in different temperature zones in the quartz tube, and after gaseous phosphorus and arsenic with high pressure in the high temperature zone (the first temperature zone) are transferred to the low temperature zone (the second temperature zone), the vapor pressure of the gaseous phosphorus and arsenic is higher than the corresponding saturated vapor pressure at the temperature of the low temperature zone, so that the dense polycrystalline arsenic or phosphorus can be obtained by desublimation, nucleation and growth of the vapor of arsenic, phosphorus and the like in the low temperature zone. Along with the continuous rise of the temperature in the quartz tube, solid phosphorus and arsenic in the high-temperature region are continuously sublimated and transferred to the low-temperature region, and then are desublimated, nucleated and grown in the low-temperature region. The end point of the migration process, namely the target temperature of heating, is that the temperature of the high-temperature zone (the first temperature zone) reaches 95-110% of the corresponding temperature of the three-phase point of the substance, and the temperature is kept for a period of time at the temperature. When arsenic, phosphorus and the like migrate from one end of the sealed quartz tube to the other end, because the pressure in the quartz tube is very high, high-boiling point impurity elements Fe, cu, si and the like in the arsenic or the phosphorus cannot volatilize and still remain in a high-temperature area, so that the separation of the arsenic, the phosphorus and high-boiling point substances is realized, and the purity of the arsenic and the phosphorus is further improved.
And after the main element is converted from the non-compact state to the compact state, the heater enters a cooling stage. And in the cooling process, the temperature difference of which the temperature is 50-100 ℃ higher than that of the second temperature zone is still kept in the first temperature zone for integral cooling until the temperature of the low-temperature zone (the second temperature zone) is more than 30 ℃ lower than the sublimation point of the substance under normal pressure, and the temperature is kept for 2-4 hours at the temperature.
And after the heat preservation is finished, the temperature difference between the high-temperature area and the low-temperature area is kept to be integrally reduced until the temperature of the high-temperature area is lower than the sublimation point of the substance by more than 50 ℃, the temperature of the lower temperature area (the second temperature area) is stopped to be reduced, the temperature of the high-temperature area is continuously reduced until the temperature of the high-temperature area is lower than the temperature of the low-temperature area by more than 100 ℃, and the temperature is synchronously reduced to the normal temperature.
The temperature of high and low temperature regions in the cooling process is controlled in order to remove the impurities of Cl and S low-boiling-point substances in non-compact arsenic and phosphorus. Cl is usually present in non-dense arsenic and phosphorus as chlorides, and is difficult to remove even with multiple water washes. And the temperature of the low-temperature area is kept higher than that of the high-temperature area in the last stage of cooling, so that volatile impurities such as Cl and S can be ensured to be finally condensed in the high-temperature area, and the separation of low-boiling point impurity elements and main elements is realized.
In the whole temperature reduction process, inert gas in the pressure container needs to be continuously discharged through the exhaust hole so as to reduce the pressure outside the quartz tube. The real-time pressure outside the quartz tube is still calculated by the Antoine equation.
The invention provides a preparation method of a compact ultra-pure material, which comprises the following steps: a) Placing the raw material in a first temperature zone of a quartz tube, heating, sublimating the raw material in a second temperature zone of the quartz tube to obtain an intermediate product; in the heating process, the temperature of the first temperature zone is 50-100 ℃ higher than that of the second temperature zone; b) Keeping the temperature difference of the first temperature zone 50-100 ℃ higher than the temperature of the second temperature zone to carry out integral cooling, firstly cooling the temperature of the second temperature zone to be 30-50 ℃ lower than the sublimation temperature of the intermediate product under normal pressure, preserving heat for 2-4 hours, and then cooling to be 50-80 ℃ lower than the sublimation temperature of the intermediate product under normal pressure; c) And stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone until the temperature of the first temperature zone is 100-120 ℃ lower than that of the second temperature zone, and finally synchronously reducing the temperatures of the first temperature zone and the second temperature zone to the normal temperature to obtain the compact ultrahigh-purity material. Compared with the existing red phosphorus/arsenic production and purification process, the whole conversion process is carried out in a closed quartz tube, the influence of the environment on the product is avoided, the temperature of the high-temperature and low-temperature regions is accurately controlled, so that the non-compact arsenic/phosphorus particles in the high-temperature region are transferred to the low-temperature region in a gaseous form, then are subjected to desublimation, nucleation and growth to obtain compact arsenic or phosphorus, and the high-boiling-point impurity elements are still left in the high-temperature region, so that the first-step purification of the arsenic/phosphorus is realized. And in the final stage of cooling, controlling the temperature of the dense arsenic or phosphorus area to be higher than that of other areas all the time, so that impurity elements such as Cl, S and the like with low boiling points are condensed at the other end, and realizing the second-step purification of arsenic/phosphorus.
In order to further illustrate the present invention, the following examples are provided to describe the preparation method of a dense ultra-high purity material, but should not be construed as limiting the scope of the present invention.
Example 1:
1000g of 5.5N red phosphorus is weighed and placed in a clean quartz tube, and the quartz tube is vacuumized and sealed.
Shaking 5.5N red phosphorus to a high temperature region, slowly pushing the quartz tube into a horizontal heater, fixing thermocouples at two ends of the quartz tube, and closing a pressure container.
And opening the control cabinet, and setting the target temperature of the high-temperature area to be 600 ℃ and the target temperature of the low-temperature area to be 550 ℃. In the temperature rise process, red phosphorus slowly changes into a gas state, fills the whole quartz tube, the pressure in the quartz tube gradually increases, the pressure P at the corresponding temperature T is calculated according to the corresponding relation of the Antoine equation lgP = A-B (T + C), the phosphorus vapor pressure P and the temperature T, and then inert gas with the pressure of P +1atm is filled into the pressure container outside the quartz tube through the gas inlet hole to ensure that the pressure outside the quartz tube is larger than the internal pressure. After reaching the set temperature, the temperature is kept for 4 hours, and the temperature of the high temperature area is ensured to be 50 ℃ higher than that of the low temperature area.
After the heat preservation is finished, the target temperature of the high-temperature area is set to be 450 ℃, and the target temperature of the low-temperature area is set
The temperature was 400 ℃. After the target temperature is reached, the temperature is preserved for 3 hours, and then the temperature is continuously reduced by the temperature difference of 50 ℃. When the temperature of the low-temperature area is reduced to 300 ℃, the low-temperature area stops cooling, the high-temperature area continues cooling to 200 ℃, and then the temperature is synchronously reduced to the normal temperature. And the temperature of the low-temperature area is kept higher than that of the high-temperature area at the last stage of cooling, so that volatile impurities such as Cl and S can be ensured to be finally condensed in the high-temperature area, and the separation of low-boiling point impurity elements and red phosphorus is realized.
When the pressure is reduced to 1bar, the pressure vessel is opened, the quartz tube is taken out, and the quartz tube cap is cut open by a quartz cutting machine to obtain 990g of compact 6N red phosphorus, wherein the yield reaches 99%.
The sample was taken for GDMS and the impurity content is shown in Table 1.
Example 2:
2000g of 7N sponge arsenic was weighed into a clean quartz tube, and the quartz tube was sealed by evacuation.
Pouring 7N arsenic to one end of the high temperature region, slowly pushing the quartz tube into the horizontal heater, and putting the quartz tube and the heating body into the pressure container;
setting the target temperature of a high-temperature area to 800 ℃, setting the target temperature of a low-temperature area to 750 ℃, wherein in the heating process, 7N arsenic is slowly changed into a gaseous state from a solid state, the whole quartz tube is filled, the pressure in the quartz tube is slowly increased, the pressure P under the corresponding temperature T is calculated according to the equation lgP = A-B (T + C), the corresponding relation between the vapor pressure P of the arsenic and the temperature T, and then inert gas with the pressure of P +1atm is filled into a pressure container outside the quartz tube through a gas inlet hole, so that the pressure outside the quartz tube is ensured to be larger than the internal pressure. When the set temperature is reached, the temperature is kept for 8 hours, and the high temperature area is ensured to be 50 ℃ higher than the low temperature area.
After the heat preservation is finished, the target temperature of the high-temperature area is set to be 650 ℃, and the target temperature of the low-temperature area is set
600 ℃, and ensuring that the high temperature area is 50 ℃ higher than the low temperature area in the period. After the target temperature is reached, the temperature is preserved for 3 hours, and then the temperature is continuously reduced by the temperature difference of 50 ℃. When the temperature of the low-temperature area is reduced to 500 ℃, the low-temperature area stops cooling, the high-temperature area continues cooling to 400 ℃, and then the temperature is synchronously reduced to the normal temperature. And the temperature of the low-temperature area is kept higher than that of the high-temperature area at the last stage of cooling, so that volatile impurities such as Cl and S can be ensured to be finally condensed in the high-temperature area, and the separation of low-boiling point impurity elements and arsenic is realized.
When the pressure is reduced to 1bar, the pressure vessel is opened, the quartz tube is taken out, and the quartz tube cap is cut open by a quartz cutter to obtain compact 7.5N arsenic 1950 with the conversion rate of 97.5%.
GDMS was sampled and examined, and the impurity contents are shown in Table 1.
Table 1 impurity levels of the products of inventive examples 1 and 2
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (3)
1. A preparation method of a compact ultrahigh-purity material comprises the following steps:
a) Placing the raw material in a first temperature zone of a quartz tube, heating, sublimating the raw material in a second temperature zone of the quartz tube to obtain an intermediate product; the quartz tube is arranged in the pressure container, and the external pressure of the quartz tube is greater than the internal pressure;
according to the relationship between the temperature and the pressure in the Antoine equation lgP = A-B (T + C) of red phosphorus and arsenic, calculating the pressure P at the corresponding temperature T, and then filling protective gas with the pressure of P +1atm into the pressure container;
in the heating process, the temperature of the first temperature zone is 50 to 100 ℃ higher than that of the second temperature zone;
b) Keeping the temperature difference between 50 and 100 ℃ higher than the temperature of the second temperature zone in the first temperature zone, carrying out overall cooling, firstly cooling the temperature of the second temperature zone to be 30 to 50 ℃ lower than the sublimation temperature of the intermediate product under normal pressure, carrying out heat preservation for 2~4 hours, and then cooling to be 50 to 80 ℃ lower than the sublimation temperature of the intermediate product under normal pressure;
c) Stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone until the temperature of the first temperature zone is 100-120 ℃ lower than that of the second temperature zone, and finally synchronously reducing the temperatures of the first temperature zone and the second temperature zone to normal temperature to obtain the compact ultra-pure material; the purity of the compact ultra-pure material is more than 99.9999%;
the raw material is arsenic or red phosphorus, and the purity of the raw material is 5N to 7N;
when the raw material is arsenic, heating to the temperature of the first temperature zone of 750-900 ℃ in the step A);
in the step B), the temperature of the first temperature zone is firstly reduced to 600-700 ℃, the temperature is preserved for 2~4 hours, and then the temperature is reduced to 500-600 ℃ of the first temperature zone;
stopping reducing the temperature of the second temperature zone, continuously reducing the temperature of the first temperature zone to 350-450 ℃, and finally synchronously reducing the temperature to the normal temperature;
when the raw material is red phosphorus, heating to the temperature of the first temperature zone of 550-700 ℃ in the step A);
in the step B), the temperature of the first temperature zone is firstly reduced to 400-500 ℃, the temperature is preserved for 2~4 hours, and then the temperature is reduced to 300-400 ℃ in the first temperature zone;
and (5) stopping reducing the temperature of the second temperature area, continuously reducing the temperature of the first temperature area to 150 to 250 ℃, and finally synchronously reducing the temperature to the normal temperature.
2. The preparation method according to claim 1, characterized in that the temperature of the first temperature zone heated in the step A) is 95-110% of the temperature corresponding to the triple point of the raw material; the heating time is 2 to 10 hours.
3. The method according to claim 1, wherein a vacuum is drawn in the quartz tube, and the pressure vessel is filled with a protective gas.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7753987B2 (en) * | 2005-09-28 | 2010-07-13 | The Chinese Academy of Sciences Institute of Physics | High vacuum in-situ refining method for high-purity materials and an apparatus thereof |
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| GB941977A (en) * | 1959-06-22 | 1963-11-20 | Monsanto Chemicals | Purification of phosphorus and arsenic |
| US3359071A (en) * | 1962-12-24 | 1967-12-19 | Siemens Ag | Method of producing hyperpure arsenic |
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