CN109704782B - Si for photovoltaic polycrystalline silicon production2N2Preparation method of O ceramic powder - Google Patents
Si for photovoltaic polycrystalline silicon production2N2Preparation method of O ceramic powder Download PDFInfo
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Abstract
The invention discloses Si for photovoltaic polycrystalline silicon production2N2The preparation method of the O ceramic powder comprises the following steps: placing the mixed powder in nitrogen atmosphere to induce the mixed powder to perform self-propagating combustion reaction to obtain Si2N2O ceramic powder; wherein the mixed powder comprises Si powder and SiO2Pulverizing; the mixed powder also comprises Si2N2O powder and/or NH4And (4) Cl powder. The invention provides Si for photovoltaic polycrystalline silicon production2N2The preparation method of the O ceramic powder utilizes the heat released by the reaction to enable the unreacted part to reach the reactable temperature so as to react, and has the characteristics of simple process, short preparation period, low energy consumption, low cost and the like.
Description
Technical Field
The present invention relates to Si2N2The technical field of O ceramic powder preparation. More particularly, it relates to a Si for photovoltaic polysilicon production2N2A preparation method of O ceramic powder.
Background
In the production process of the photovoltaic polycrystalline silicon ingot, the ceramic crucible is a key material, silicon materials are melted in the crucible, crystal grows, annealing and cooling are carried out, the silicon materials are cast into a polycrystalline silicon ingot, the silicon ingot is cut into silicon wafers according to requirements, and the silicon ingot can be used for manufacturing solar cells. At present, a quartz ceramic crucible is used in the production of photovoltaic polycrystalline silicon ingots. Silicon melt and quartz crucible take place the reaction under high temperature, lead to the impurity element to get into and pollute silicon melt on the one hand, on the other hand reaction leads to silicon melt and quartz crucible adhesion, and silicon ingot casting and crucible take place the fracture when leading to the drawing of patterns, seriously influence the quality and the productivity promotion of polycrystalline silicon ingot casting. Therefore, a method of coating a silicon nitride coating on the surface of the quartz crucible is generally used to prevent the reaction between the silicon melt and the quartz crucible and to reduce the loss caused during the mold release. Nevertheless, the quartz crucible is difficult to reuse in the actual production process, which results in an increase in the production cost of photovoltaic polycrystalline silicon.
From the point of view of micromachine, Si (l) + SiO occurs at high temperature in the silicon melt and quartz2(s) → 2sio (g) deoxidation attack the crucible and the expansion behavior of the silicon melt during cooling causes silicon intrusion into the crucible pits and large stresses resulting in sticking and cracking of the silicon ingot to the quartz crucible. After the silicon nitride coating is used, the weak interface of the porous structure of the layer slows down the corrosion of the silicon melt to the quartz crucible. Essentially, the silicon melt is on SiO2The contact angle of the matrix is 85 degrees, and the matrix is not wetted; to Si3N4The contact angle of the substrate was 49 deg., and was wet. Naturally occurring thin SiO layer on the surface of silicon nitride material2The film is the key point that the porous silicon nitride coating and silicon melt show non-wettability and slow down the erosion of the quartz crucible. And the thin layer of SiO2The film, which disappears as the deoxidation reaction proceeds, causes the silicon melt to change from non-wetting to wetting and eventually to penetrate the coating to erode the crucible. Therefore, the adoption of the ceramic material which is not wetted to the silicon melt eliminates a deoxidation reaction path, solves the problems of adhesion and cracking of the silicon ingot and the crucible, and is a necessary way for improving the quality and yield of the photovoltaic polycrystalline silicon and reducing the production cost.
From the material system, the ceramic crucible material for photovoltaic polysilicon not only has excellent high-temperature mechanical and thermal properties, but also needs to not introduce impurities and not to be wetted with silicon melt, which limits the selectable range of the material, wherein Si is Si2N2O-ceramics is one possible choice. Si2N2The O ceramic is a high-performance high-temperature structural ceramic and has excellent high-temperature strength, thermal shock resistance, thermal stability and oxidation resistance. However, in the prior art, Si2N2The O ceramic is mainly prepared through high-temperature in-situ reaction, and the process has high energy consumption, long period and high cost and limits the scale application of the O ceramic.
Therefore, the invention provides Si for photovoltaic polycrystalline silicon production2N2A preparation method of O ceramic powder to solve the problems.
Disclosure of Invention
An object of the present invention is to provide Si for photovoltaic polysilicon production2N2A preparation method of O ceramic powder. The method solves the problem of Si in the prior art2N2The production cost of the O ceramic powder is high; produced Si2N2The O ceramic powder can be used for preparing a ceramic crucible and a demoulding coating for producing photovoltaic polycrystalline silicon, solves the problems of adhesion and cracking of a silicon ingot and the crucible, and improves the quality and yield of silicon ingots.
In order to achieve the purpose, the invention adopts the following technical scheme:
si for photovoltaic polycrystalline silicon production2N2The preparation method of the O ceramic powder comprises the following steps:
placing the mixed powder in nitrogen atmosphere to induce the mixed powder to perform self-propagating combustion reaction to obtain Si2N2O ceramic powder;
wherein the mixed powder comprises Si powder and SiO2Pulverizing; the mixed powder also comprises Si2N2O powder and/or NH4And (4) Cl powder.
Preferably, the mixed powder comprises the following components in parts by weight:
35-56 parts of Si powder;
SiO225-40 parts of powder;
Si2N2the content of the O powder is more than 0 part and not more than 40 parts.
Preferably, the mixed powder comprises the following components in parts by weight:
35-56 parts of Si powder;
SiO225-40 parts of powder;
NH4the Cl powder is more than 0 part and not more than 4 parts.
Preferably, the mixed powder comprises the following components in parts by weight:
preferably, the mixed powder is placed in a high-pressure combustion synthesis device for self-propagating combustion reaction.
Preferably, the specific way of inducing the mixed powder to generate the high-temperature reaction is to use a spiral tungsten wire to electrify and generate heat to induce the mixed powder to generate a self-propagating combustion reaction.
Preferably, the pressure of the nitrogen is 1-4 MPa.
Preferably, in the mixed powder, the Si powder and the SiO powder2The weight ratio of the powder was 1.4: 1.
In addition, unless otherwise specified, any range recited herein includes any value between the endpoints and any sub-range defined by any value between the endpoints or any value between the endpoints.
The invention has the following beneficial effects:
the invention provides Si for photovoltaic polycrystalline silicon production2N2The preparation method of the O ceramic powder utilizes the heat released by the reaction to enable the unreacted part to reach the reactable temperature so as to react, and has the characteristics of simple process, short preparation period, low energy consumption, low cost and the like.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows Si obtained in example 1 of the present invention2N2SEM photograph of O ceramic powder.
FIG. 2 shows the silicon melt vs. Si in example 2 of the present invention2N2High temperature contact angle photo of the O coating.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
In the invention, the preparation method is a conventional method if no special description is provided; the starting materials used are, unless otherwise specified, commercially available from published sources; the percentages are mass percentages unless otherwise specified.
In the prior art, Si2N2The O ceramic is mainly prepared by high-temperature in-situ reaction, and the high-temperature in-situ reaction usually requires heating the raw materials to 1500 ℃ and carrying out long-time heat preservation to prepare Si2N2O, the process has high energy consumption, long period and high cost, and the scale application of the process is limited. In order to solve the above problems, the present invention provides Si2N2The preparation method of the O ceramic powder utilizes the heat released by the reaction to ensure that the unreacted part reaches the reactable temperature to react, thereby reducing the required energy consumption, and the reaction process is simple and has short period.
Particularly, the invention provides Si for photovoltaic polycrystalline silicon production2N2The preparation method of the O ceramic powder comprises the following steps: placing the mixed powder in nitrogen atmosphere to induce the mixed powder to perform self-propagating combustion reaction to obtain Si2N2O ceramic powder; wherein the mixed powder comprises Si powder and SiO powder in parts by weight2Pulverizing; the mixed powder also comprises Si2N2O powder and/or NH4And (4) Cl powder. The invention can obtain Si only by inducing the mixed powder to generate self-propagating combustion reaction2N2The O ceramic powder has simple reaction process, does not need high-temperature heating, long-time heat preservation and the like; in addition, the invention utilizes the heat released by inducing the mixed powder to carry out high-temperature reaction to ensure that the unreacted part of the powder reaches the reactable temperature so as to continue the reaction, thereby reducing the required energy consumption and further reducing the production cost; further, the mixed powder removes Si powder and SiO2In addition to the powder, Si is also added2N2O powder and/or NH4Cl powder to solve the problem of Si2N2Si impurity phase and SiO in O ceramic powder2Hetero phase and Si3N4More impurities.
As a preferred embodiment, the mixed powder is placed in a high-pressure combustion synthesis device to carry out self-propagating combustion reaction.
As a preferred embodiment, the mixed powder comprises, in parts by weight:
35-56 parts of Si powder;
SiO225-40 parts of powder;
Si2N2the content of the O powder is more than 0 part and not more than 40 parts. When Si is contained in the mixed powder2N2Weight portion of O powder>At 40 parts, Si is present in the product3N4A heterogeneous phase exists.
As a preferred embodiment, the mixed powder comprises, in parts by weight:
35-56 parts of Si powder;
SiO225-40 parts of powder;
NH4the Cl powder is more than 0 part and not more than 4 parts. When NH is contained in the mixed powder4Cl powder weight portion>When 4 parts are used, Si is contained in the product3N4A heterogeneous phase exists.
As a preferred embodiment, the mixed powder comprises, in parts by weight:
35-56 parts of Si powder;
SiO225-40 parts of powder;
Si2N2more than 0 part and not more than 40 parts of O powder;
NH4the Cl powder is more than 0 part and not more than 4 parts. When the mixed powder contains Si2N2O powder and NH4When Cl powder is used, the product Si is reduced2N2Si impurity phase and SiO in O ceramic powder2Hetero phase and Si3N4The presence of a heterogeneous phase.
Specifically, the specific way of inducing the mixed powder to generate the high-temperature reaction is to adopt a spiral tungsten wire to electrify and generate heat to induce the mixed powder to generate a self-propagating combustion reaction.
Further, the pressure of the nitrogen is 1-4 MPa; a large number of experiments prove that the performance effect of the obtained product is optimal within the pressure range, and the product performance is reduced when the pressure exceeds the range.
Further, in the mixed powder, the Si powder and SiO powder2The weight ratio of the powder is 1.4: 1; the skilled person of the invention has proved through a large number of experiments thatUnder the condition of the weight ratio, the obtained product has the optimal performance effect, and under the condition of the weight ratio, the product Si2N2No Si impurity phase and SiO existing in the O ceramic powder2Hetero phase and Si3N4And (3) impurity phase.
Example 1
Si2N2The preparation of the O ceramic powder comprises the following steps:
35g of Si powder, 25g of SiO2Powder and 40g of Si2N2Mixing O powder uniformly to obtain mixed powder; in high-pressure combustion synthesis equipment in nitrogen atmosphere of 4MPa, a spiral tungsten wire is adopted to be electrified and heated to induce the mixed powder to carry out self-propagating combustion reaction, and Si is obtained2N2O ceramic powder.
XRD test is carried out on the obtained ceramic powder, and the result shows that the component of the product is Si2N2O, no impurity phase is generated; SEM test of the obtained ceramic powder shows that the product has uniform particle size distribution, as shown in figure 1; preparing the obtained powder into a ceramic coating, coating the ceramic coating on the surface of a quartz substrate, performing a high-temperature seat drop experiment, and measuring the Si ratio of the silicon melt to Si2N2The contact angle of the O-coating was 120 °.
Example 2
Si2N2The preparation of the O ceramic powder comprises the following steps:
42g of Si powder and 30g of SiO2Powder, 27g of Si2N2O powder and 1g of NH4Uniformly mixing Cl powder to obtain mixed powder; in high-pressure combustion synthesis equipment in nitrogen atmosphere of 3MPa, a spiral tungsten wire is adopted to be electrified and heated to induce the mixed powder to carry out self-propagating combustion reaction, and Si is obtained2N2O ceramic powder.
XRD test is carried out on the obtained ceramic powder, and the result shows that the component of the product is Si2N2O, no impurity phase is generated; SEM test is carried out on the obtained ceramic powder, and the result shows that the product has uniform granularity distribution; preparing the obtained powder into a ceramic coating, coating the ceramic coating on the surface of a quartz substrate, performing a high-temperature seat drop experiment, and measuring the Si ratio of the silicon melt to Si2N2O coatingThe contact angle of the layer is 120 deg., as shown in fig. 2.
Example 3
Si2N2The preparation of the O ceramic powder comprises the following steps:
49g of Si powder, 35g of SiO2Powder, 13g of Si2N2O powder and 3g of NH4Cl powder is evenly mixed to obtain mixed powder; in high-pressure combustion synthesis equipment in 2MPa nitrogen atmosphere, a spiral tungsten wire is adopted to be electrified and heated to induce the mixed powder to carry out self-propagating combustion reaction to obtain Si2N2O ceramic powder.
XRD test is carried out on the obtained ceramic powder, and the result shows that the component of the product is Si2N2O, no impurity phase is generated; SEM test is carried out on the obtained ceramic powder, and the result shows that the product has uniform granularity distribution; preparing the obtained powder into a ceramic coating, coating the ceramic coating on the surface of a quartz substrate, performing a high-temperature seat drop experiment, and measuring the Si ratio of the silicon melt to Si2N2The contact angle of the O-coating was 120 °.
Example 4
Si2N2The preparation of the O ceramic powder comprises the following steps:
56g of Si powder, 40g of SiO2Powder and 4g of NH4Cl powder is evenly mixed to obtain mixed powder; in high-pressure combustion synthesis equipment in 1MPa nitrogen atmosphere, a spiral tungsten wire is adopted to be electrified and heated to induce the mixed powder to carry out self-propagating combustion reaction to obtain Si2N2O ceramic powder.
XRD test is carried out on the obtained ceramic powder, and the result shows that the component of the product is Si2N2O, no impurity phase is generated; SEM test is carried out on the obtained ceramic powder, and the result shows that the product has uniform granularity distribution; preparing the obtained powder into a ceramic coating, coating the ceramic coating on the surface of a quartz substrate, performing a high-temperature seat drop experiment, and measuring the Si ratio of the silicon melt to Si2N2The contact angle of the O-coating was 120 °.
Some examples of the invention
In order to examine the influence of the mixed powder formula on the chemical composition of the product, the method steps are carried out simultaneouslyExample 1, only Si powder and SiO powder in the mixed powder were changed2Powder, Si2N2O powder and NH4The amount and ratio of Cl powder are shown in the following table.
TABLE 1 results for different raw material ratios
| Example numbering | Si powder/g | SiO2Powder/g | Si2N2O powder/g | NH4Cl powder/g | Chemical composition of the product |
| 5 | 58.3 | 41.7 | 0 | 0 | Si2N2O、Si3N4、Si |
| 6 | 36 | 24 | 40 | 0 | Si2N2O、Si |
| 7 | 34 | 26 | 40 | 0 | Si2N2O、SiO2 |
| 8 | 33.6 | 24 | 42.4 | 0 | Si2N2O、SiO2 |
| 9 | 31.5 | 22.5 | 42 | 4 | Si2N2O、Si3N4 |
| 10 | 55.4 | 39.6 | 0 | 5 | Si2N2O、Si3N4 |
The results show that: when the mixed powder is not added with Si2N2O powder and NH4When Cl powder is used, Si and Si are contained in the product3N4The presence of a heterogeneous phase; when Si is SiO in the mixed powder2>1.4:1, Si impurity phase exists in the product; when Si is SiO in the mixed powder2<At 1.4:1, there is SiO in the product2The presence of a heterogeneous phase; when Si is contained in the mixed powder2N2Weight portion of O powder>At 40 parts, Si is present in the product3N4The presence of a heterogeneous phase; when NH is contained in the mixed powder4Cl powder weight portion>When 4 parts are used, Si is contained in the product3N4A heterogeneous phase exists. When Si is SiO in the mixed powder21.4:1, and Si powder and SiO powder in the mixed powder2Powder, Si2N2O powder and NH4When the Cl powder is used in the range given in the invention, the component of the product is Si2N2O, no impurity phase is generated.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (5)
1. Si for photovoltaic polycrystalline silicon production2N2The preparation method of the O ceramic powder is characterized by comprising the following steps:
placing the mixed powder in nitrogen atmosphere to induce the mixed powder to perform self-propagating combustion reaction to obtain Si2N2O ceramic powder;
the mixed powder comprises the following components in parts by weight:
35-56 parts of Si powder;
SiO225-40 parts of powder;
NH4the Cl powder is more than 0 part and not more than 4 parts;
or, the mixed powder comprises the following components in parts by weight:
35-56 parts of Si powder;
SiO225-40 parts of powder;
Si2N2more than 0 part and not more than 40 parts of O powder;
NH4the Cl powder is more than 0 part and not more than 4 parts.
2. Si for photovoltaic polysilicon production according to claim 12N2The preparation method of the O ceramic powder is characterized in that the mixed powder is placed in high-pressure combustion synthesis equipment for self-propagating combustion reaction.
3. Si for photovoltaic polysilicon production according to claim 12N2The preparation method of the O ceramic powder is characterized in that the specific mode of inducing the mixed powder to generate the self-propagating combustion reaction is to adopt a spiral tungsten wire to electrify and generate heat to induce the mixed powder to generate the self-propagating combustion reaction.
4. Si for photovoltaic polysilicon production according to claim 12N2The preparation method of the O ceramic powder is characterized in that the pressure of the nitrogen is 1-4 MPa.
5. Si for photovoltaic polysilicon production according to claim 12N2The preparation method of the O ceramic powder is characterized in that in the mixed powder, the Si powder and the SiO powder2The weight ratio of the powder was 1.4: 1.
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| CN111960828A (en) * | 2020-08-03 | 2020-11-20 | 武汉科技大学 | Silicon oxynitride/quartz composite ceramic crucible for smelting photovoltaic silicon and preparation method thereof |
| CN114477781A (en) * | 2020-10-23 | 2022-05-13 | 中国科学院理化技术研究所 | Preparation process of composite ceramic coating release agent |
| CN114684797B (en) * | 2022-03-08 | 2023-10-13 | 中国科学院过程工程研究所 | Preparation of pure-phase multi-shell Si 2 N 2 System and method for O-hollow spherical powder |
| CN116851630B (en) * | 2023-08-15 | 2024-04-05 | 上海勘测设计研究院有限公司 | Slurry for casting and demolding as well as preparation method and application thereof |
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