CN115573025A - Method for growing artificial quartz crystal raw material for high-purity quartz sand with purity of more than 5N - Google Patents
Method for growing artificial quartz crystal raw material for high-purity quartz sand with purity of more than 5N Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 171
- 239000013078 crystal Substances 0.000 title claims abstract description 156
- 239000010453 quartz Substances 0.000 title claims abstract description 120
- 239000002994 raw material Substances 0.000 title claims abstract description 48
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000005520 cutting process Methods 0.000 claims abstract description 31
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 230000007797 corrosion Effects 0.000 claims abstract description 11
- 238000005260 corrosion Methods 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims description 19
- 230000008025 crystallization Effects 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 11
- 239000004576 sand Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 7
- 239000011707 mineral Substances 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 4
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000003814 drug Substances 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 3
- 150000002500 ions Chemical class 0.000 abstract description 6
- 239000006184 cosolvent Substances 0.000 abstract description 4
- 238000001953 recrystallisation Methods 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000002173 cutting fluid Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000010423 industrial mineral Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/18—Quartz
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for growing artificial quartz crystal raw materials for high-purity quartz sand of more than 5N, which comprises the steps of completing seed crystal preparation by seed crystal cutting and seed crystal corrosion, completing sorting by adopting natural quartz, adding mineralizer solution into a reaction kettle as a cosolvent, dissolving the natural quartz in the reaction kettle for recrystallization under the conditions of high temperature and high pressure, lifting the reaction kettle into a kettle pit, controlling the temperature, and stably growing quartz crystals in the kettle pit to obtain the artificial quartz crystal raw materials for preparing the high-purity quartz sand; in particular to three links of seed crystal preparation, natural quartz separation and crystal growth. The invention adopts natural quartz as a raw material for preparing high-purity quartz sand, removes impurity ions in the natural quartz crystal by purifying the raw material of the natural quartz crystal, and greatly improves the utilization rate of quartz ore and the purity of quartz sand in China.
Description
Technical Field
The invention belongs to the field of preparation of high-purity quartz sand raw materials, and particularly relates to a method for growing an artificial quartz crystal raw material for high-purity quartz sand with the purity of more than 5N.
Background
The quartz sand is a nonmetallic mineral substance, is milk-white in color, is a hard, wear-resistant and chemically stable silicate mineral, and has the main mineral component of SiO 2 (ii) a The quartz sand is an important industrial mineral raw material, and has high temperature resistance, excellent chemical characteristics, excellent electrical insulation and light transmission; the high-purity quartz sand is mainly applied to the fields of semiconductors, photovoltaics, optical communication and electric light sources, and is an irreplaceable mineral raw material for high and new technology industries. Quartz is the main raw material for producing quartz sand and is one of the most widely distributed minerals on the earth surface; although the quartz ore is rich in raw material reserves, the impurities are various and unstable in property, and are gradually exhausted due to the increase of mining intensity; the search for high-quality quartz sand made of high-purity quartz is a necessary requirement of the current industrial production.
The high-purity quartz sand with the grade of 4N8 or above is a key raw material for manufacturing semiconductor monocrystalline silicon, effectively removes impurity components in quartz ore raw materials, improves the quality and the utilization rate of quartz, and solves the problem that no ore is available.
Disclosure of Invention
Aiming at the problems existing in the preparation of the existing high-purity quartz sand raw material, the invention provides a method for growing an artificial quartz crystal raw material for high-purity quartz sand with the purity of more than 5N; the invention adopts a hydrothermal temperature difference method, natural quartz is dissolved in a reaction kettle under a high-temperature and high-pressure environment and then is recrystallized, thereby removing most impurity ions in the quartz, eliminating gas-liquid inclusions in the natural quartz, reducing solid inclusions and meeting the requirement of preparing the artificial quartz crystal raw material for high-purity quartz sand.
A growth method of artificial quartz crystal raw material for high-purity quartz sand with the purity of more than 5N comprises the steps of completing seed crystal preparation through seed crystal cutting and seed crystal corrosion, completing sorting by adopting natural quartz, adding a mineralizer into a reaction kettle as a cosolvent, dissolving the natural quartz in the reaction kettle under the conditions of high temperature and high pressure for recrystallization, lifting the reaction kettle into a kettle pit, controlling the temperature, and stably growing the quartz crystal in the kettle pit to obtain the artificial quartz crystal raw material for preparing the high-purity quartz sand; in particular to three links of seed crystal preparation, natural quartz separation and crystal growth, comprising the following steps:
(1) Completing the seed crystal preparation in the previous stage by seed crystal cutting and seed crystal corrosion; cutting the seed crystal by using a multi-wire cutting machine, cleaning the seed crystal after the cutting is finished, and punching two holes on two ends of the seed crystal in the length direction; putting the cleaned seed crystal into a corrosion machine for corrosion to achieve the purposes of removing the processing stress and the damaged layer;
(2) Sorting natural quartz by using domestic quartz ores;
(3) 0.8mol/L NaOH and 0.4mol/L Na are adopted 2 CO 3 0.05mol/L of NaNO 3 Preparing a mineralizer solution by using 0.05mol/L LiOH solution, and calculating the dosage of the prepared mineralizer;
(4) Calculating the yield of a single kettle, the seed crystal demand and the natural quartz consumption;
(5) Putting seed crystals, natural quartz and a mineralizer solution into a reaction kettle, dissolving the natural quartz in a dissolving area, and convecting to a crystallization area through a baffle plate, wherein the dissolved natural quartz forms a supersaturated solution due to the reduction of temperature, and the supersaturated solution is crystallized on the seed crystals;
(6) And (3) hoisting the reaction kettle into the kettle pit, stably controlling the growth conditions of the quartz crystal through a temperature control instrument, and after the crystallization process is finished, growing the quartz crystal to form an artificial quartz crystal to obtain the raw material for preparing the high-purity quartz sand.
Preferably, the cutting angle of the multi-wire cutting machine in the step (1) is set to be 20 degrees +/-2 degrees, the width of the wire casing is set to be 1.1mm, the cutting speed is set to be 0.15 mm/min, the sand liquid in the multi-wire cutting machine is silicon carbide sand GC1000 and water cutting liquid, and the sand liquid proportion is set to be 1:1.
Preferably, the solution in the etching machine in the step (1) is 30% ammonium bifluoride solution, the temperature is set to be 60 +/-1 ℃, the etching amount is 0.1mm, and the etching time is set to be 30min.
Preferably, the natural quartz granularity in the step (2) is 2-4cm 2 The content is more than or equal to 99.5 percent, the total content of metal impurities is less than or equal to 80ppm, wherein the AI content is less than or equal to30ppm, fe content less than or equal to 15ppm, ca content less than or equal to 18ppm, no iron rust, no mica, no oil stain and no mineral skin on the appearance, clean particle surface, and neutral water quality after being soaked in pure water.
Preferably, the chemicals in step (3) are used in the following process, and dissolved by pure water to form mineralizer solution:
volume of solution: v Solution ＝(V Kettle -V Quartz -V Seed crystal -V Crystal frame )*X％
The filling quality of the medicine is as follows: n = V Solution *C*Mr
Wherein V Solution : volume of solution charged, V Kettle : effective volume of the kettle, V Quartz : volume of quartz, V Seed crystal : charged seed crystals product, V Crystal frame : the volume of the boule, all volume units are liters, X%: the solution filling degree is generally 82-84%, N: chemical charge, C: molar concentration of chemical charge, mr: molecular weight of the chemical.
Preferably, the calculation processes of the single-kettle yield of the reaction kettle, the seed crystal demand and the natural quartz dosage in the step (4) are as follows:
calculating the yield of a single kettle: m Crystal ＝V Kettle *a
Calculating seed crystal requirements: n is a radical of Seed crystal ＝M Crystal Artificial quartz crystal raw material single block weight
Calculating the using amount of the natural quartz: m Quartz ＝M Crystal *1.25
Wherein M is Crystal : design yield (per kilogram) of raw material for artificial quartz crystal, V Kettle : autoclave volume (unit liter), a: the yield coefficient takes a value of 0.55; n is a radical of Seed crystal : number of seed crystals (unit piece), M Crystal : the yield (unit kilogram) of the artificial quartz crystal raw material is designed, the X-direction size of the seed crystal is 70mm, and the Y-direction length is 200-210mm, and the average single weight of each artificial quartz crystal raw material is 1.2 kilograms.
Preferably, an autoclave with the caliber of 240-400mm is selected as the reaction kettle in the step (5), and the pressure in the autoclave is more than or equal to 140MPa.
Preferably, the reaction kettle in the step (5) is bounded by a baffle, a dissolving area is arranged below the baffle, and natural quartz, pure water and a mineralizer are filled in the reaction kettle; a crystallization area is arranged above the baffle and is provided with seed crystals (including a crystal frame); the heating temperature of the dissolution zone was set to 380 ℃ and the heating temperature of the crystallization zone was set to 340 ℃.
Preferably, the crystallization area is provided with a seed crystal and a crystal frame, and an iron wire penetrates through two holes at the end part of the seed crystal and is tied on the seed crystal frame.
Preferably, the quartz crystal growth conditions in the step (6) are that double baffles are adopted in the reaction kettle, and the aperture ratio of the baffles is 4-8%; the growth temperature of the crystallization area is set to be 340 ℃, the growth period is set to be 50 days, and the growth size can reach 25-30mm.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts natural quartz as a raw material for preparing high-purity quartz sand, removes impurity ions in the quartz crystal by purifying the quartz crystal raw material, and greatly improves the utilization rate of the natural quartz.
(2) The high-purity quartz sand with the purity of more than 5N prepared by the invention has the advantages of low bubble content, less impurity ions and stable chemical property, and can completely replace American Union melt import quartz sand to be used for the inner layer of a semiconductor crucible.
Detailed Description
In order that the invention may be better understood, the invention will now be further described with reference to specific examples. The following examples are given to illustrate the detailed embodiments and operation procedures based on the technology of the present invention, but the scope of the present invention is not limited to the following examples.
The invention relates to a method for growing artificial quartz crystal raw materials for high-purity quartz sand of more than 5N, which adopts a hydrothermal temperature difference method, particularly relates to three links of seed crystal preparation, natural quartz sorting and crystal growth, and aims to remove most impurity ions in natural quartz, eliminate gas-liquid inclusions in natural quartz, reduce solid inclusions and meet the requirements for preparing the raw materials for the high-purity quartz sand of 5N and more.
The design idea of the invention is as follows: cutting and seeding through seed crystalCrystal etching is carried out to complete the preparation of the seed crystal, wherein the length of the seed crystal is 200-210mm, the width is 70-80mm, the thickness is 0.9 +/-0.1 mm, GC1000 sand or finer sand is used for cutting the seed crystal, and a seed crystal etching tunnel is less than or equal to 30 strips/cm 2 (ii) a Then the domestic quartz ore is adopted to complete the natural quartz separation, and the separation condition is set as SiO 2 The content is more than or equal to 99.5 percent, the total content of metal impurities is less than or equal to 80ppm, wherein the AI content is less than or equal to 30ppm, the Fe content is less than or equal to 15ppm, the Ca content is less than or equal to 18ppm, the selected quartz has the granularity of 2-4cm, no iron rust, no mica, no oil stain and no mineral skin on the appearance, the particle surface is clean, and the water quality is neutral after being soaked in pure water; adding a mineralizer as a cosolvent into a reaction kettle, wherein the reaction kettle is a high-pressure kettle with the caliber of 240-400mm, and the set pressure is more than or equal to 140MPa; dissolving natural quartz in a reaction kettle under the conditions of high temperature and high pressure for recrystallization, lifting the reaction kettle into a kettle pit, controlling the temperature difference between a dissolving area and a crystallizing area to be 40 ℃ by adopting double baffles, and setting the aperture ratio of the baffles to be 4-8% so that the dissolved natural quartz is in normal convection in the dissolving area and the crystallizing area; and the dissolved natural quartz convects to enter a crystallization area to form supersaturated solution, the supersaturated solution is crystallized on seed crystals, and quartz crystals stably grow in the kettle pits to obtain the artificial quartz crystal raw material for preparing the high-purity quartz sand.
The following example is an implementation process of a technical scheme of the method for growing the artificial quartz crystal raw material for the high-purity quartz sand with the purity of more than 5N, and the method comprises the following specific operation steps:
step 1: cutting seed crystals; cutting seed crystals by using a multi-wire cutting machine, wherein the cutting angle is 20 +/-2 degrees, the cutting speed is 0.15 mm/min, and the width of a wire groove is 1.1mm; the ratio of the carborundum sand GC1000 to the water cutting fluid in the multi-wire cutting machine is 1:1, and the seed crystal is continuously ground by the sand fluid under the drive of the steel wire to achieve the effect similar to cutting; after cutting, cleaning the attached cutting fluid and cutting sand; two holes with the diameter of 1mm are respectively drilled at the two ends of the seed crystal in the length direction, so that the seed crystal is conveniently bound on the seed crystal frame by using iron wires.
And 2, step: seed crystal corrosion; putting the cleaned seed crystal into 30% ammonium bifluoride solution and a corrosion machine with the temperature of 60 +/-1 ℃ to corrode for 30 minutes, wherein the corrosion amount is 0.1mm; the purpose of removing the processing stress and the damage layer is achieved.
And step 3: calculating the feeding amount; the method specifically comprises the following substeps:
substep 3.1: the calculation process of the single kettle yield is M Crystal ＝V Kettle *a
Wherein M is Crystal : design yield (in kg), V Kettle : the autoclave volume (in liters), a is the yield coefficient, the Z-direction thickness of the product is 20-30mm, and the yield coefficient is 0.55.
Substep 3.2: the calculation process of seed crystal requirement is N Seed crystal ＝M Crystal Artificial quartz crystal raw material single block weight
Wherein N is Seed crystal : number of seed crystals (unit piece), M Crystal : the yield (unit kilogram) of the artificial quartz crystal raw material is designed, the X-direction size of the seed crystal is 70mm, and the Y-direction size of the seed crystal is 200-210mm, and the average single weight of each artificial quartz crystal raw material is 1.2 kilograms.
Substep 3.3: the calculation process of the natural quartz dosage is M Quartz ＝M Crystal *1.25。
Substep 3.4: the preparation and calculation process of the mineralizer are as follows, the mineralizer selects 0.8mol/L NaOH and 0.4mol/L Na 2 CO 3 0.05mol/L of NaNO 3 And 0.05mol/L LiOH solution, calculating the specific dosage of chemicals according to the following formula, mixing and preparing, and dissolving by using pure water to form a mineralizer solution.
Volume of mineralizer solution is V Solution ＝(V Kettle -V Quartz -V Seed crystal -V Crystal frame )*X％
The filling quality of the medicine is as follows: n = V Solution *C*Mr
Wherein V Solution : volume of solution charged, V Kettle : effective volume of the kettle, V Quartz : volume of quartz, V Seed crystal : charged seed crystals product, V Crystal frame : the volume of the boule, all volume units are liters, X%: the solution filling degree is generally 82-84%, N: chemical charge (in grams), C: molar concentration of chemical charge, mr: division of chemicalsAnd (4) sub-quantities.
And 4, step 4: hanging seed crystals; the special seed crystal frame is utilized, the seed crystal is tied on the seed crystal frame through the iron wire, and the seed crystal provides a center which is easy for the crystal to continue growing so as to promote the formation of the quartz crystal.
And 5: cleaning natural quartz; washing the selected qualified quartz with tap water to remove dust on the surface, soaking in pure water for more than 4 hours, and measuring the conductivity of water to be less than 25 mus/cm.
Step 6: filling into a kettle; injecting pure water into the kettle, simultaneously gradually pouring weighed and cleaned quartz, then adding the prepared mineralizer solution, and continuously injecting water to V Solution Until the end; taking a baffle as a boundary, loading natural quartz, pure water and a mineralizer below the baffle, wherein a dissolving area is arranged below the baffle, a seed crystal (containing a crystal frame) is arranged above the baffle, and a crystallization area is arranged above the baffle; the heating temperature of the dissolving area is set to 380 ℃, the heating temperature of the crystallization area is set to 340 ℃, the dissolved natural quartz flows to the crystallization area through the baffle, a supersaturated solution is formed due to the reduction of the temperature, the supersaturated solution is crystallized on the seed crystal, and the quartz crystal grows into an artificial quartz crystal.
And 7: hoisting the reaction kettle into a kettle pit; the temperature of a dissolving zone and the temperature of a crystallization zone are controlled to be constant through a temperature control instrument, natural quartz in the dissolving zone is dissolved under the action of high temperature, high pressure and a cosolvent, a supersaturated solution is formed after the natural quartz enters the crystallization zone through convection, the supersaturated solution is crystallized on seed crystals, the growth of quartz crystals lasts for 50 days, the growth temperature is stably controlled to be 340 ℃, the temperature difference between the dissolving zone and the crystallization zone is 40 ℃, the growth size of the quartz crystals reaches 25-30mm under the pressure of 140MPa, and the artificial quartz crystal raw material for preparing the high-purity quartz sand is obtained.
And 8: taking out the raw materials from the kettle, and taking out the artificial quartz crystal raw materials in the kettle; the components of the raw material of the artificial quartz crystal were measured, and the results were as follows (unit PPm):
AI(3.2)；B(＜0.04)；Ca(0.37)；Co(＜0.01)；Cu(0.01)；Fe(0.09)； K(0.17)；Li(0.88)；Mg(0.13)；Mn(0.01)；Na(1.68)；Ni(＜0.02)； Ti(＜0.02)。
the process of this embodiment through accomplishing the natural quartz of selecting separately and dissolving the recrystallization under reation kettle high temperature high pressure reaches and gets rid of AI in the natural quartz, most impurity ions such as Li, na, K, fe, obtains the artificial quartz crystal raw materials of preparation high-purity quartz sand.
The invention can have other forms of embodiment according to the above method, which are not listed. Therefore, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention by those skilled in the art can be made within the technical scope of the present invention.
Claims (10)
1. A method for growing a raw material of an artificial quartz crystal for high-purity quartz sand with the purity of more than 5N is characterized by relating to three links of seed crystal preparation, natural quartz separation and crystal growth, and specifically comprises the following steps:
(1) Completing the seed crystal preparation in the previous stage by seed crystal cutting and seed crystal corrosion; cutting the seed crystal by using a multi-wire cutting machine, cleaning the seed crystal after cutting, punching two holes at two ends of the seed crystal in the length direction, and putting the seed crystal into a corrosion machine for corrosion;
(2) Sorting natural quartz by using domestic quartz ores;
(3) 0.8mol/L NaOH and 0.4mol/L Na are adopted 2 CO 3 0.05mol/L of NaNO 3 Preparing a mineralizer solution by using 0.05mol/L LiOH solution, and calculating the dosage of the prepared mineralizer;
(4) Calculating the yield of a single kettle, the seed crystal demand and the natural quartz consumption;
(5) Putting seed crystals, natural quartz and a mineralizer solution into a reaction kettle, dissolving the natural quartz in a dissolving region, and convecting to a crystallization region through a baffle plate, wherein the dissolved natural quartz forms a supersaturated solution due to the reduction of temperature, and the supersaturated solution is crystallized on the seed crystals;
(6) And (3) hoisting the reaction kettle into a kettle pit, stably controlling the crystal growth conditions through a temperature control instrument, and after the crystallization process is finished, growing the quartz crystal to form an artificial quartz crystal to obtain the raw material for preparing the high-purity quartz sand.
2. The method for growing the artificial quartz crystal raw material for the high-purity quartz sand of more than 5N according to claim 1, wherein the cutting angle of the multi-wire cutting machine in the step (1) is set to 20 degrees +/-2 degrees, the wire casing width is set to 1.1mm, the cutting speed is set to 0.15 mm/min, the sand liquid in the multi-wire cutting machine is selected from silicon carbide sand GC1000 and water cutting liquid, and the sand liquid proportion is set to 1:1.
3. The method for growing an artificial quartz crystal material for use in 5N or more high purity quartz sand according to claim 1, wherein the solution in the etching machine in the step (1) is a 30% strength ammonium bifluoride solution, the temperature is set to 60 ℃ ± 1 ℃, the etching amount is 0.1mm, and the etching time is set to 30min.
4. The method for growing a raw material of artificial quartz crystal for quartz sand of 5N or more high purity according to claim 1, wherein the natural quartz is sorted under the following conditions in the step (2): the granularity of the natural quartz is 2-4cm 2 The content is more than or equal to 99.5 percent, the total content of metal impurities is less than or equal to 80ppm, wherein the AI content is less than or equal to 30ppm, the Fe content is less than or equal to 15ppm, the Ca content is less than or equal to 18ppm, the natural quartz has no iron rust, mica, oil stain and mineral skin, the particle surface is clean, and the water quality is neutral after being soaked in pure water.
5. The method for growing an artificial quartz crystal material for 5N or more high purity quartz sand according to claim 1, wherein the chemicals used in the step (3) are dissolved in pure water to form a mineralizer solution in an amount calculated by the following procedure:
volume of solution: v Solution ＝(V Kettle -V Quartz -V Seed crystal -V Crystal frame )*X％
The filling quality of the medicine is as follows: n = V Solution *C*Mr
Wherein V Solution : volume of solution charged, V Kettle : effective volume of the kettle, V Quartz : volume of quartz, V Seed crystal : volume of seed crystals charged, V Crystal frame : volume of the crystal frame, all volume unitsIn liters, X%: the solution filling degree is generally 82-84%, N: chemical charge amount, C: molar concentration of chemical charge, mr: molecular weight of the chemical.
6. The method for growing a raw material of artificial quartz crystal for high-purity quartz sand of 5N or more according to claim 1, wherein the calculation process of the single-pot yield of the reaction pot, the required amount of seed crystal and the used amount of natural quartz in the step (4) is as follows:
calculating the yield of a single kettle: m Crystal ＝V Kettle *a
Calculating seed crystal requirements: n is a radical of Seed crystal ＝M Crystal Artificial quartz crystal raw material single block weight
Calculating the using amount of the natural quartz: m Quartz ＝M Crystal *1.25
Wherein M is Crystal : design yield (per kilogram) of raw material for artificial quartz crystal, V Kettle : autoclave volume (unit liter), a: the yield coefficient takes a value of 0.55; n is a radical of Seed crystal : number of seed crystals (unit piece), M Crystal : the yield (in kilograms) of the synthetic quartz crystal feedstock is designed.
7. The method for growing a raw material of artificial quartz crystal for high-purity quartz sand of 5N or more according to claim 1, wherein an autoclave with a bore of 240-400mm is selected as the reaction vessel in the step (5), and the pressure in the autoclave is 140MPa or more.
8. The method for growing an artificial quartz crystal raw material for 5N or more high-purity quartz sand according to claim 1, wherein the reaction kettle of the step (5) is bounded by a baffle below which a dissolution zone is arranged, and natural quartz, pure water and a mineralizer are filled; a crystallization area is arranged above the baffle and is provided with seed crystals and a crystal frame; the heating temperature of the dissolution zone was set to 380 ℃ and the heating temperature of the crystallization zone was set to 340 ℃.
9. The method for growing an artificial quartz crystal material for use in 5N or more high purity quartz sand according to claim 8, wherein said crystallization zone is provided with a seed crystal and a seed holder, and wherein said seed crystal is passed through two holes formed in the end of said seed crystal by means of a wire and is bound to said seed holder.
10. The method for growing the artificial quartz crystal raw material for the high-purity quartz sand of more than 5N according to claim 1, wherein the quartz crystal growth conditions in the step (6) are that double baffles are adopted in the reaction kettle, and the aperture ratio of the baffles is 4-8%; the growth temperature of the crystallization area is set to be 340 ℃, the growth period is set to be 50 days, and the growth size can reach 25-30mm.
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| CN117051476A (en) * | 2023-10-11 | 2023-11-14 | 北京石晶光电科技股份有限公司 | High-purity quartz sand prepared by utilizing artificial quartz crystal |
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