Preparation method and device of diiodosilane

Abstract

The invention relates to a preparation method and device of diiodosilane, and relates to the field of synthesis methods of semiconductor materials, the preparation method comprises the following steps: 1, mixing and dissolving iodine with at least one of chloroform, dichloromethane and dichloroethane according to a volume ratio of 1: (2-5); the phenylsilane is mixed with at least one of ethyl acetate, tert-butyl acetate and butyl acetate according to the mass ratio of 100: (1-5); pre-cooling the iodine solution and the phenylsilane solution at-40 to 0 DEG C; then pumping the mixture into a microchannel reactor, carrying out mixed reaction for 100-300 seconds in a low-temperature microchannel at-40-10 DEG C, and then introducing the mixture into a room-temperature microchannel at 20-30 DEG C to react for 100-400 seconds, so as to obtain a reaction mixture; and 2, carrying out vacuum rectification on the reaction mixture obtained in the step 1, and collecting the product with the fraction temperature of 35-40 DEG C under 20 + / -3 mmHg to obtain the high-purity diiodosilane. The diiodosilane is synthesized through the microchannel reactor, the original synthesis period can be shortened to be within 700 seconds, and the obtained mixture product is high in content and low in impurity metal ion content.

Description

technical field

[0001] The invention relates to the field of synthesis methods of semiconductor materials, in particular to a preparation method and device of diiodosilane. Background technique

[0002] High-purity diiodosilane plays an increasingly important role in high-end semiconductor chips. As a silicon source for chemical vapor deposition, it can pass gas-phase reaction CVD (Chemical VaporDeposition) at lower temperature and more controllable pressure operation. and ALD (atomic layer deposition) methods to deposit silicide films on a wide variety of semiconductor substrates. Diiodosilane has attracted wide attention due to its unique advantages and broad market prospects. However, the existing high-purity diiodosilane synthesis method is complicated and dangerous, which severely limits the industrialization of the product, and the application direction determines that its purity requirements are very high, and the preparation of 99.9999+% effective purity product is ...

Examples

Embodiment 1

[0046] Example 1: Chloroform is a solvent for iodine

[0047] Under nitrogen protection, a homogeneous mixed solution containing 3518.1 g of iodine and 10 L of chloroform was prepared. At the same time, a mixed solution of 1500 g of phenylsilane and 58.8 ml of ethyl acetate was pumped into the microchannel reactor respectively. 8:1, after pre-cooling at -40°C, the mixture was simultaneously passed through a low temperature microchannel at -35°C and a room temperature microchannel at +25°C, and the residence time was 200s and 300s, respectively, to obtain a mixture. The mixture was rectified to obtain 3625 g of a colorless liquid, 92.11%. The calculation method is as follows: 3625 / (1500*283.91 / 108.21)*100%=92.11%.

[0048] Using the GC chromatographic area normalization method, the purity of diiodosilane was 99.9+%, as shown in Table 1 and figure 2 shown.

[0049] Purity calculation of the diiodosilane of Table 1 Example 1

[0050]

Embodiment 2

[0051] Example 2: Chloroform is a solvent for iodine

[0052] Under nitrogen protection, a homogeneous mixed solution containing 3518.1 g of iodine and 10 L of chloroform was prepared. At the same time, a mixed solution of 1500 g of phenylsilane and 58.8 ml of ethyl acetate was pumped into the microchannel reactor respectively. The volume flow ratio of the iodine solution and the phenylsilane solution was 8 : 1. After pre-cooling at -20°C, the mixture was obtained by passing through the -15°C low temperature microchannel and the room temperature microchannel at +25°C, respectively, with the residence time of 200s and 300s. The mixture was rectified to obtain 3683 g of a colorless liquid, 93.58%. Using the GC chromatographic area normalization method, the purity of diiodosilane is greater than 99.9+%, as shown in Table 2 and image 3 shown.

[0053] The purity calculation of the diiodosilane of table 2 embodiment 2

[0054]

Embodiment 3

[0055] Example 3: Chloroform is a solvent for iodine

[0056] Under nitrogen protection, a homogeneous mixed solution containing 3518.1 g of iodine and 10 L of chloroform was prepared. At the same time, a mixed solution of 1500 g of phenylsilane and 58.8 ml of ethyl acetate was pumped into the microchannel reactor respectively. The volume flow ratio of the iodine solution and the phenylsilane solution was 10 : 1. After being pre-cooled at 0°C, the mixture is obtained by passing through a low temperature microchannel at 10°C and a room temperature microchannel at +25°C, respectively, for a residence time of 100s and 300s. The mixture was rectified to obtain 3541 g of a colorless liquid, 89.97%. Using GC chromatographic area normalization method, the purity of diiodosilane is greater than 99.9+%, as shown in Table 3 and Figure 4 shown.

[0057] The purity calculation of the diiodosilane of table 3 embodiment 3

[0058]

[0059] From Example 1, Example 2, and Example 3, it...

technical field

[0001] The invention relates to the field of synthesis methods of semiconductor materials, in particular to a preparation method and device of diiodosilane. Background technique

[0002] High-purity diiodosilane plays an increasingly important role in high-end semiconductor chips. As a silicon source for chemical vapor deposition, it can pass gas-phase reaction CVD (Chemical VaporDeposition) at lower temperature and more controllable pressure operation. and ALD (atomic layer deposition) methods to deposit silicide films on a wide variety of semiconductor substrates. Diiodosilane has attracted wide attention due to its unique advantages and broad market prospects. However, the existing high-purity diiodosilane synthesis method is complicated and dangerous, which severely limits the industrialization of the product, and the application direction determines that its purity requirements are very high, and the preparation of 99.9999+% effective purity product is ...

Examples

Embodiment 1

[0046] Example 1: Chloroform is a solvent for iodine

[0047] Under nitrogen protection, a homogeneous mixed solution containing 3518.1 g of iodine and 10 L of chloroform was prepared. At the same time, a mixed solution of 1500 g of phenylsilane and 58.8 ml of ethyl acetate was pumped into the microchannel reactor respectively. 8:1, after pre-cooling at -40°C, the mixture was simultaneously passed through a low temperature microchannel at -35°C and a room temperature microchannel at +25°C, and the residence time was 200s and 300s, respectively, to obtain a mixture. The mixture was rectified to obtain 3625 g of a colorless liquid, 92.11%. The calculation method is as follows: 3625 / (1500*283.91 / 108.21)*100%=92.11%.

[0048] Using the GC chromatographic area normalization method, the purity of diiodosilane was 99.9+%, as shown in Table 1 and figure 2 shown.

[0049] Purity calculation of the diiodosilane of Table 1 Example 1

[0050]

Embodiment 2

[0051] Example 2: Chloroform is a solvent for iodine

[0052] Under nitrogen protection, a homogeneous mixed solution containing 3518.1 g of iodine and 10 L of chloroform was prepared. At the same time, a mixed solution of 1500 g of phenylsilane and 58.8 ml of ethyl acetate was pumped into the microchannel reactor respectively. The volume flow ratio of the iodine solution and the phenylsilane solution was 8 : 1. After pre-cooling at -20°C, the mixture was obtained by passing through the -15°C low temperature microchannel and the room temperature microchannel at +25°C, respectively, with the residence time of 200s and 300s. The mixture was rectified to obtain 3683 g of a colorless liquid, 93.58%. Using the GC chromatographic area normalization method, the purity of diiodosilane is greater than 99.9+%, as shown in Table 2 and image 3 shown.

[0053] The purity calculation of the diiodosilane of table 2 embodiment 2

[0054]

Embodiment 3

[0055] Example 3: Chloroform is a solvent for iodine

[0056] Under nitrogen protection, a homogeneous mixed solution containing 3518.1 g of iodine and 10 L of chloroform was prepared. At the same time, a mixed solution of 1500 g of phenylsilane and 58.8 ml of ethyl acetate was pumped into the microchannel reactor respectively. The volume flow ratio of the iodine solution and the phenylsilane solution was 10 : 1. After being pre-cooled at 0°C, the mixture is obtained by passing through a low temperature microchannel at 10°C and a room temperature microchannel at +25°C, respectively, for a residence time of 100s and 300s. The mixture was rectified to obtain 3541 g of a colorless liquid, 89.97%. Using GC chromatographic area normalization method, the purity of diiodosilane is greater than 99.9+%, as shown in Table 3 and Figure 4 shown.

[0057] The purity calculation of the diiodosilane of table 3 embodiment 3

[0058]

[0059] From Example 1, Example 2, and Example 3, it...

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