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Refining method of tetra (dimethylamino) hafnium

A technology of dimethylamino and purification methods, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, and organic compounds of Group 4/14 without C-metal bonds, etc., and can resolve Hf elements and Zr It is difficult to separate elements, the products cannot meet the purity requirements of the electronics industry for the use of products, and it is difficult to prepare high-purity products, etc., to achieve the effects of less investment, low equipment requirements, and simple operation

Pending Publication Date: 2021-05-11
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there is no domestic literature report on the refining method of this compound, and the product obtained by the conventional distillation method cannot meet the purity requirements of the electronic industry for the product.
.Currently the main problem is the difficulty of separating Hf element and Zr element, and it is difficult to prepare 99.9% high-purity products

Method used

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  • Refining method of tetra (dimethylamino) hafnium
  • Refining method of tetra (dimethylamino) hafnium
  • Refining method of tetra (dimethylamino) hafnium

Examples

Experimental program
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Effect test

Embodiment 1

[0029] A method for refining tetrakis(dimethylamino) hafnium, the specific scheme is as follows:

[0030] Add 80g of tetrakis(dimethylamino)hafnium crude product into the refining reaction kettle, add 0.5g of adsorption resin under the protection of nitrogen, control the temperature at 30°C, stir and mix for 20min, filter and remove the adsorption resin, and then add tetrakis(dimethylamino)hafnium crude product Import it into a still, control the temperature at 10°C, remove the volatile components under reduced pressure, then raise the temperature to 80°C, and distill under reduced pressure to obtain the refined tetrakis(dimethylamino)hafnium product.

[0031] Described adsorption resin is a kind of surface graft modified adsorption resin, and its preparation method is:

[0032] Use an electron accelerator to irradiate 50g of D101 polystyrene macroporous adsorption resin with electron beams to generate active free radicals that can be used for grafting reactions. Irradiation c...

Embodiment 2

[0036] A method for refining tetrakis(dimethylamino) hafnium, the specific scheme is as follows:

[0037] Add 100g of tetrakis(dimethylamino)hafnium crude product into the refining reaction kettle, add 1.2g of adsorption resin under the protection of nitrogen, control the temperature at 35°C, stir and mix for 50min, filter and remove the adsorption resin, and then add tetrakis(dimethylamino)hafnium crude product Import it into a distillation kettle, control the temperature at 30°C, remove the volatile components under reduced pressure, then raise the temperature to 60°C, and distill under reduced pressure to obtain the refined tetrakis(dimethylamino)hafnium product.

[0038] Described adsorption resin is a kind of surface graft modified adsorption resin, and its preparation method is:

[0039] Use an electron accelerator to irradiate 60g of polystyrene macroporous adsorption resin with electron beams to generate active free radicals that can be used for grafting reactions. Irr...

Embodiment 3

[0043] A method for refining tetrakis(dimethylamino) hafnium, the specific scheme is as follows:

[0044] Add 120g of tetrakis(dimethylamino)hafnium crude product into the refining reaction kettle, add 3g of adsorption resin under the protection of nitrogen, control the temperature at 40°C, stir and mix for 90min, filter and remove the adsorption resin, and then introduce tetrakis(dimethylamino)hafnium crude product into Put it into a still, control the temperature at 35°C, remove the volatile components under reduced pressure, then raise the temperature to 50°C, and distill under reduced pressure to obtain the refined tetrakis(dimethylamino)hafnium product.

[0045] Described adsorption resin is a kind of surface graft modified adsorption resin, and its preparation method is:

[0046] Use an electron accelerator to irradiate 70g of polystyrene macroporous adsorption resin with electron beams to generate active free radicals that can be used for grafting reactions. Irradiation...

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Abstract

The invention relates to the field of chemical engineering, and particularly relates to a refining method of tetra (dimethylamino) hafnium. The method comprises the steps of firstly, carrying out refined adsorption on a tetra (dimethylamino) hafnium crude product by adopting surface grafting modified adsorption resin to remove a small amount of reaction raw material dimethylamine and a reaction byproduct n-butyl alcohol contained in the product, then firstly removing a trace amount of volatile impurities of residual reaction raw materials at low temperature by adopting a reduced pressure distillation mode, and then heating and distilling to obtain a high-purity product. The method has the advantages that the operation is simple, the equipment requirement is low, the investment is low, the prepared product has high purity, and the purity requirement on the tetra (dimethylamino) hafnium compound product in the electronic industry can be met.

Description

technical field [0001] The invention relates to the field of chemical engineering, in particular to a method for refining tetrakis(dimethylamino)hafnium. Background technique [0002] Tetrakis(dimethylamino)hafnium is mainly used for making below 28nm, and is mainly used in the formation of HfN film in copper shielding applications and the fabrication of HKMG electrodes. HKMG (high-k insulating layer + metal gate) technology has almost become an essential technology for processes below 45nm. [0003] CN102760758A discloses a metal gate structure, which includes a high dielectric constant gate dielectric layer, a nitrogen-containing layer, a work function metal layer, and a nitrogen trapping layer. The nitrogen-containing layer is disposed between the work function metal layer and the high dielectric constant gate dielectric layer; and the nitrogen trapping layer is disposed between the work function metal layer and the high dielectric constant gate dielectric layer between...

Claims

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Application Information

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IPC IPC(8): C07F7/00C08F257/02C08F230/06C08F212/14C08F226/02B01J20/30B01J20/26
CPCC07F7/003C08F257/02B01J20/264C08F230/065C08F212/22C08F226/02
Inventor 贺辉龙李军张广第朱世雷徐琴琪张晓东花永紧徐建仙
Owner ZHEJIANG BRITECH CO LTD
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