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Method for synthesizing hafnocene dichloride

A technology of hafnium dichloride and a synthesis method is applied in the synthesis field of metal-organic complexes to achieve the effects of improving product purity, changing reaction temperature and simplifying conditions

Inactive Publication Date: 2012-01-18
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Purpose of the invention: the present invention mainly aims at the defects of the synthesis method of dichlorodicene-based hafnium in the prior art, and provides an improved synthesis method

Method used

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Experimental program
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Embodiment 1

[0014] Synthesis of hafnocene dichloride

[0015] (1) Depolymerize cyclopentadiene under a nitrogen atmosphere, and collect the distilled cyclopentadiene monomer at 40-42° C. into a flask cooled by an ice-water bath for subsequent use.

[0016] (2) Under the protection of a pure nitrogen atmosphere, add 69g of sodium wire cut into small pieces and 450mL of diethylene glycol dimethyl ether into a 1000mL three-necked bottle, stir mechanically, and slowly heat to 120-160°C until the sodium is completely melted Uniformly disperse in diethylene glycol dimethyl ether in the form of sodium sand, add 270mL of freshly prepared cyclopentadiene dropwise into a three-necked bottle, reflux and stir for 4 hours after the dropwise addition, until the sodium is completely reacted, under nitrogen protection Cool down to room temperature.

[0017] (3) 481 grams of hafnium tetrachloride are added to a three-necked bottle filled with 500 milliliters of normal hexane, and the diethylene glycol di...

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Abstract

The invention relates to a method for synthesizing hafnocene dichloride, which comprises the following process steps: depolymerizing cyclopentadiene: depolymerizing the cyclopentadiene under inert atmosphere, and collecting cyclopentadiene monomers obtained by distillation for standby; heating a solvent of diglycol ether and sodium wires under the inert atmosphere, then dripping the cyclopentadiene monomers, carrying out reaction after completing the dripping, and obtaining diglycol ether solution of cyclopentadienyl sodium; dripping the well prepared cyclopentadienyl sodium solution into n-hexane suspension of hafnium tetrachloride solids, and carrying out reaction at the temperature of 15-35 DEG C; firstly removing the n-hexane under one atmospheric pressure, further removing the diglycol ether, obtaining dark gray solids, carrying out extraction on the solids by using a Soxhlet extractor, filtrating extraction solution, depressurizing, removing the solvent by evaporation, cooling, then precipitating the solids, and obtaining a target product. The method firstly improves the dispersion of sodium, thereby improving the yield of the produced cyclopentadienyl sodium; and then the reaction is carried out with the solid hafnium tetrachloride in the suspension in the solvent, thereby obtaining the target product with higher efficiency.

Description

1. Technical field [0001] The invention relates to a method for synthesizing metal-organic complexes in the field of chemistry. 2. Background technology [0002] With the continuous development of the semiconductor manufacturing industry, high-k and metal gate material precursors suitable for ALD and CVD are found through continuous comparison of material properties. For the 32nm technology node, issues such as material volatility, transport mode, and purity become critical. As the amount of information stored and retrieved has increased dramatically, so has the need for higher-k materials, which can be found in any available element from alumina to rare metals. [0003] Research has found that when the gate oxide thickness is less than 2nm, the leakage current will be greatly increased, and high dielectric constant materials can allow thicker gate dielectric materials, thereby reducing leakage current and becoming necessary; choosing appropriate high-k materials can meet ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/00
Inventor 潘毅韩建林孔令宇曹季虞磊
Owner NANJING UNIV
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