CN111943215A - Preparation method of quartz powder - Google Patents
Preparation method of quartz powder Download PDFInfo
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- CN111943215A CN111943215A CN201910399619.7A CN201910399619A CN111943215A CN 111943215 A CN111943215 A CN 111943215A CN 201910399619 A CN201910399619 A CN 201910399619A CN 111943215 A CN111943215 A CN 111943215A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C01P2006/80—Compositional purity
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Abstract
The invention provides a preparation method of quartz powder, which comprises the following steps: the preset volume ratio of SiCl4Carrying out hydrolysis reaction with water to obtain silicic acid gel with a space network structure, and then aging; drying the surface moisture of the silicic acid gel and the moisture in the structural gaps at a first temperature range for the next time to obtain a material 1; drying the material 1 for the second time at a second temperature interval to dehydrate to obtain a material 2; and calcining the material 2 to obtain quartz powder. The invention adopts SiCl4And water is used as a main raw material, so that the introduction of other impurities is avoided, the agglomeration phenomenon of powder is prevented by a multi-time drying technology, the moisture is fully eliminated, the hydroxyl content is reduced, and the high-purity quartz powder is prepared.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method of quartz powder.
Background
This section is intended to provide a background or context to the embodiments of the invention that are recited in the claims. The description herein is not admitted to be prior art by inclusion in this section.
The quartz sand is mainly applied to the industries of IC integrated circuits, quartz glass and the like, and high-grade products of the quartz sand are more widely applied to the fields of large-scale and super-large-scale integrated circuits, optical fibers, lasers, aerospace, military and the like. With the increasing demand for the purity of quartz sand in the fields of crucibles for semiconductors, integrated circuits, and the like, the problems of uneven purity, resource exhaustion, and the like of natural quartz sand are gradually eliminated, and the development of high-purity synthetic quartz powder is urgently needed.
The existing preparation of high-purity quartz powder comprises the steps of preparing synthetic quartz powder by using water glass as a raw material, and removing alkali metal ions by using cation exchange resin; and the synthetic quartz powder is prepared by using alkoxy silane as a raw material, but carbon element is easily introduced, which may cause generation of bubbles. In the methods, alkoxy silane or water glass is used as a raw material, so that impurities such as carbon element or alkali metal ions can be introduced, and quartz glass is easy to generate bubbles or has low viscosity; and on the other hand, the impurity removal process is complex.
Disclosure of Invention
In view of the above, there is a need for an improved method for preparing quartz powder.
The technical scheme provided by the invention is as follows: a preparation method of quartz powder comprises the following steps:
the preset volume ratio of SiCl4Carrying out hydrolysis reaction with water to obtain silicic acid gel with a space network structure, and then aging;
drying the surface moisture of the silicic acid gel and the moisture in the structural gaps at a first temperature range for the next time to obtain a material 1;
drying the material 1 for the second time at a second temperature interval to dehydrate to obtain a material 2;
and calcining the material 2 to obtain quartz powder.
Further, the temperature range of the first temperature interval is 100-300 ℃.
Further, the step of drying the water in the gaps of the silicic acid gel structure at the first temperature range for the next time to obtain the material 1 comprises:
and drying the surface moisture of the silicic acid gel and 70-90% of filling moisture in the structural gaps at the first temperature range for 1-20h to obtain a material 1.
Further, the temperature range of the second temperature interval is 700-1000 ℃.
Further, the step of drying the material 1 for the second time at the second temperature interval to dehydrate and obtain the material 2 includes:
the time range of the secondary drying is 1-10h, and the moisture in the dehydration comprises the balance of filling moisture and reaction water eliminated by hydroxyl.
Further, the SiCl4And water in a volume ratio ranging from 1:3 to 1: 12.
Further, the aging time range is 10-50 h.
Further, the duration of the calcination ranges from 0.5 to 10 hours. The calcination step serves to eliminate pores in the gel and densify it.
Further, the step of calcining the material 2 to obtain quartz powder comprises the following steps:
and calcining the material 2 in a vacuum atmosphere to obtain quartz powder.
Further, the gas pressure control range in the calcining process is 10-100 Pa.
Compared with the prior art, the preparation method of the quartz powder provided by the invention adopts SiCl4The raw material avoids the introduction of other impurities, and the agglomeration phenomenon of powder is prevented by a multi-time drying technology, so that the moisture is fully eliminated, the hydroxyl content is reduced, and the high-purity quartz powder is prepared.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a flow chart illustrating the preparation of quartz powder according to an embodiment of the present invention.
Description of reference numerals:
none.
The following detailed description further illustrates embodiments of the invention in conjunction with the above-described figures.
Detailed Description
So that the manner in which the above recited objects, features and advantages of embodiments of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings. In addition, the features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth to provide a thorough understanding of embodiments of the invention, and the described embodiments are merely a subset of embodiments of the invention, rather than a complete embodiment. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the embodiments of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which embodiments of the present invention belong. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the invention.
Referring to fig. 1, a process for preparing quartz powder according to a preferred embodiment of the present invention mainly comprises the following steps:
step S1: the preset volume ratio of SiCl4And carrying out hydrolysis reaction with water to obtain silicic acid gel with a space network structure, and then aging.
In this embodiment, the SiCl4The volume ratio of the water to the water is 1:3-1: 12; the aging time range is 10-50 h. Wherein the water is selected to focus on the reaction water with low impurity ion content, especially the metal ion should be ppb level, as long as the concentration requirement of the impurity ion is met, such as deionized water, distilled water and the like.
Step S2: and drying the water on the surface of the silicic acid gel and in the structural gap at the first temperature range for the next time to obtain a material 1.
In this embodiment, step S2 is specifically to perform a first drying of the surface moisture of the silicic acid gel and 70 to 90% of the filling moisture in the structural voids at a first temperature range, where the duration of the first drying is in a range of 1 to 20 hours, so as to obtain material 1. Wherein the temperature range of the first temperature interval is 100-300 ℃. The aim of the step is to avoid agglomeration of the calcined quartz powder.
Step S3: and drying the material 1 for the second time at a second temperature interval to dehydrate to obtain a material 2.
In this embodiment, the temperature range of the second temperature zone is 700 to 1000 ℃. The time range of the secondary drying is 1-10h, and the moisture in the dehydration comprises the balance of filling moisture and reaction water eliminated by hydroxyl.
Step S4: and calcining the material 2 to obtain quartz powder.
In the present embodiment, the time period of the calcination is in the range of 0.5 to 10 hours. The calcination step serves to eliminate pores in the gel and densify it. Step S4 is specifically to calcine the material 2 in vacuum atmosphere to obtain quartz powder, wherein the air pressure control range in the calcining process is 10-100 Pa.
The above steps can not be reversed, SiCl is adopted4And water is used as a raw material, impurities such as carbon element or alkali metal and the like cannot be introduced in the production process, and the drying in multiple steps is indispensable, wherein the primary drying function is to remove free water and bound water on the surface of the gel and in the gaps at low temperature, the water in the gaps is called as filling water in the embodiment, and the water in the pore diameter of the gel is slowly dried at low temperature, so that the gel can be prevented from being broken to generate agglomeration; secondary drying is used for removing hydroxyl (-OH) and organic matters in the gel structure to realize the purification of quartz powder; the effect of calcination is to eliminate pores in the gel and densify it. The quartz powder prepared by the method has high purity, and meets the application requirements in the fields of crucibles for semiconductors, integrated circuits and the like; and the process steps are simplified, thereby being beneficial to large-scale industrial production.
The following examples illustrate the preparation of the quartz powder of the present invention and the product properties.
Comparative example
Mixing SiCl with the volume ratio of 1:34Hydrolyzing with deionized water to obtain silicic acid gel, aging for 15h, oven drying at 700 deg.C for 2h, calcining at 100Pa and 1400 deg.C for 1h to obtain high purity synthetic quartz powder, and showing that the quartz powder is obtainedThe powder was heavily agglomerated.
Example 1
Mixing SiCl with the volume ratio of 1:34Hydrolyzing with deionized water to obtain silicic acid gel, aging for 15h, oven drying at 300 deg.C for 1h, oven drying at 700 deg.C for 10h, and calcining at 100Pa and 1400 deg.C for 0.5h to obtain high purity synthetic quartz powder with no agglomeration, and measured to obtain metal impurity content of 0.08ppm and hydroxyl content of 50 ppm.
Example 2
Mixing SiCl with the volume ratio of 1:64Hydrolyzing with deionized water to obtain silicic acid gel, aging for 60h, oven drying at 150 deg.C for 6h, oven drying at 800 deg.C for 6h, calcining at 80Pa and 1200 deg.C for 8h to obtain non-agglomerated high-purity synthetic quartz powder with metal impurity content of 0.2ppm and hydroxyl content of 30 ppm.
Example 3
Mixing SiCl with the volume ratio of 1:84Hydrolyzing with deionized water to obtain silicic acid gel, aging for 100h, oven drying at 120 deg.C for 10h, oven drying at 900 deg.C for 3h, and calcining at 1300 deg.C under 10Pa for 3h to obtain high purity synthetic quartz powder with no agglomeration, and metal impurity content of 0.5ppm and hydroxyl content of 10 ppm.
Example 4
Mixing SiCl with the volume ratio of 1:124Hydrolyzing with deionized water to obtain silicic acid gel, aging for 150h, oven drying at 100 deg.C for 20h, oven drying at 1000 deg.C for 1h, and calcining at 1350 deg.C under 10Pa for 1.5h to obtain high purity synthetic quartz powder with no agglomeration, metal impurity content of 0.99ppm and hydroxyl content of 8 ppm.
Example 5
Mixing SiCl with the volume ratio of 1:34Hydrolyzing with deionized water to obtain silicic acid gel, aging for 15h, oven drying at 120 deg.C for 4h, oven drying at 700 deg.C for 2h, and calcining at 100Pa and 1400 deg.C for 1h to obtain high purity synthetic quartz powder without agglomeration and with metal impurity content0.98ppm and a hydroxyl group content of 50 ppm.
Example 6
Mixing SiCl with the volume ratio of 1:54Hydrolyzing with deionized water to obtain silicic acid gel, aging for 60h, oven drying at 150 deg.C for 2h, oven drying at 800 deg.C for 3h, and calcining at 80Pa and 1350 deg.C for 2h to obtain high purity synthetic quartz powder without agglomeration, with metal impurity content of 0.5ppm and hydroxyl content of 30 ppm.
Example 7
Mixing SiCl with the volume ratio of 1:64Hydrolyzing with deionized water to obtain silicic acid gel, aging for 100h, oven drying at 200 deg.C for 1h, oven drying at 900 deg.C for 2h, and calcining at 1300 deg.C under 10Pa for 3h to obtain high purity synthetic quartz powder without agglomeration, with metal impurity content of 0.09ppm and hydroxyl content of 10 ppm.
In other embodiments, SiCl4The volume ratio to water, the aging time, the primary drying temperature, the primary drying time, the secondary drying temperature, the secondary drying time, the calcination air pressure, the calcination temperature, the calcination time, and the like are not limited to the above embodiments; and the multi-step drying can also be three-step drying or more than three steps, so that the high-purity quartz powder is not agglomerated, the calcining process is more sufficient, and the like.
In conclusion, the quartz powder formed by the method of the invention has no agglomeration phenomenon and high purity, the content of metal impurities is approximately 0.08-0.99ppm, the content of hydroxyl groups is 8-50ppm, and the content of metal impurities is 0.09ppm and the content of hydroxyl groups is 10ppm under the optimal conditions. Moreover, the method has the advantages of simplified steps, strong operability and high batch production efficiency.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (10)
1. The preparation method of the quartz powder is characterized by comprising the following steps of:
the preset volume ratio of SiCl4Carrying out hydrolysis reaction with water to obtain silicic acid gel with a space network structure, and then aging;
drying the surface moisture of the silicic acid gel and the moisture in the structural gaps at a first temperature range for the next time to obtain a material 1;
drying the material 1 for the second time at a second temperature interval to dehydrate to obtain a material 2;
and calcining the material 2 to obtain quartz powder.
2. The method for producing a quartz powder according to claim 1, characterized in that: the temperature range of the first temperature interval is 100-300 ℃.
3. The method for preparing quartz powder according to claim 1, wherein the step of drying the water in the voids of the silicic acid gel structure at a first temperature range to obtain a material 1 comprises:
and drying the surface moisture of the silicic acid gel and 70-90% of filling moisture in the structural gaps at the first temperature range for 1-20h to obtain a material 1.
4. The method for producing a quartz powder according to claim 1, characterized in that: the temperature range of the second temperature interval is 700-1000 ℃.
5. The method for preparing quartz powder according to claim 3, wherein the step of drying the material 1 for the second time at the second temperature interval to dehydrate the material to obtain the material 2 comprises:
the time range of the secondary drying is 1-10h, and the moisture in the dehydration comprises the balance of filling moisture and reaction water eliminated by hydroxyl.
6. The method for producing a silica powder according to claim 1, characterized in thatCharacterized in that: the SiCl4And water in a volume ratio ranging from 1:3 to 1: 12.
7. The method for producing a quartz powder according to claim 1, characterized in that: the aging time range is 10-50 h.
8. The method for producing a quartz powder according to claim 1, characterized in that: the duration of the calcination ranges from 0.5 to 10 hours.
9. The method for producing a silica powder as claimed in claim 1, wherein the step of calcining the material 2 to obtain a silica powder comprises:
and calcining the material 2 in a vacuum atmosphere to obtain quartz powder.
10. The method for producing a quartz powder according to claim 9, characterized in that: the air pressure control range in the calcining process is 10-100 Pa.
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| CN201910399619.7A CN111943215B (en) | 2019-05-14 | 2019-05-14 | Preparation method of quartz powder |
| PCT/CN2019/094787 WO2020228115A1 (en) | 2019-05-14 | 2019-07-05 | Quartz powder and preparation method therefor |
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| CN201910399619.7A CN111943215B (en) | 2019-05-14 | 2019-05-14 | Preparation method of quartz powder |
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