Preparation method of high-density ultrafine particle graphite for ionization chamber

A technology of ultra-fine particles and ionization chambers, which is applied in the field of high-density ultra-fine particle graphite preparation for ionization chambers. The materials can not meet the problems, so as to achieve the effect of promoting industrialization, reducing the difficulty of roasting, and improving the interface bonding

Active Publication Date: 2021-04-30
中国人民解放军96901部队23分队
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] As a world-class carbon R&D and production company, SGL Group aims to provide the highest-end graphite, but it is still unable to achieve the size enlargement of ultra-fine graphite. / 8650” ultra-fine graphite, the standard blank size of the product is only 610mm×390mm×190mm / 1230mm×480mm×260mm, it is difficult to purchase graphite of this size in China, and the price is expensive
The ZXF-5Q of POCO in the United States and the HPG-510 of Toyo Tanso in Japan can both achieve high density and high strength, but it is even more difficult to obtain products that are larger than 150mm in three directions in China.
[0006] In summary, the traditional graphite production process route has been unable to meet the preparation process requirements of ultra-fine graphite, which seriously restricts the preparation and wide application of materials.
At present, the performance of ordinary carbon / graphite materials can no longer meet the requirements of special fields, especially graphite materials for nuclear reactors, aerospace and large-scale air ionization chambers. It is urgent to develop the preparation of ultra-fine particles and high-density carbon / graphite materials that are easy to scale up. Program

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  • Preparation method of high-density ultrafine particle graphite for ionization chamber
  • Preparation method of high-density ultrafine particle graphite for ionization chamber

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preparation example Construction

[0033] figure 1 It is a schematic flow chart of the preparation method of high-density ultra-fine particle graphite for ionization chambers according to an embodiment of the present invention, as figure 1 Shown, the preparation method of the ionization chamber provided by the invention uses highly dense ultra-fine particle graphite, comprises the following steps:

[0034] Step S1, crushing the coal tar pitch, stirring with the first organic solvent at a temperature of 50-100°C, extracting the insoluble matter, drying the solvent, crushing the insoluble matter again, and mixing it with the second organic solvent at a temperature of 50-100°C Fully stirred under the condition to obtain the soluble matter solution;

[0035] Wherein, the softening point of the coal tar pitch is 70-270°C.

[0036] In one embodiment of the present invention, the bitumen and insoluble matter can be crushed into pieces with a size of 20-50 μm.

[0037] In one embodiment of the present invention, the...

Embodiment 1

[0062] Crush the coal tar pitch with a softening point of 270°C to 20 μm and stir it with toluene at 50°C for 30 minutes, extract the insoluble matter, dry the solvent, crush it again to 20 μm, and stir it with quinoline solvent at 50°C for 30 minutes. A soluble solution was obtained. When the temperature of the pitch coke with an average particle size of 1 μm in the kneader reaches 120°C, add the soluble matter solution dissolved in quinoline solvent as a binder into the kneader for liquid phase mixing for 1 hour, and the binder accounts for 35%. Then the temperature was raised to 260°C for 1 hour, and the solvent was evaporated to obtain a paste. The paste was crushed to 5 μm to obtain pressed powder. Put the pressed powder into a mold at 200 MPa and press to form, keep the pressure for 30 minutes, and release the pressure to make a green sample. The green body sample is carbonized in argon, the heating rate is 2°C / min, the final carbonization temperature is 1000°C, and th...

Embodiment 2

[0064] Crush the coal tar pitch with a softening point of 80°C to 50 μm and stir it with acetone at 100°C for 120 minutes, extract the insoluble matter, dry the solvent, crush it again to 50 μm, and stir it with pyridine solvent at 100°C for 120 minutes to obtain Soluble solution. When the temperature of the pitch coke with an average particle size of 15 μm in the kneader reaches 50°C, add the soluble matter solution dissolved in pyridine solvent as a binder into the kneader for liquid phase mixing for 3 hours, the binder accounts for 25%, and then The temperature was raised to 140°C for 3 hours, and the solvent was evaporated to obtain a paste. The paste was crushed to 50 μm to obtain pressed powder. Put the pressed powder into a mold at 120 MPa and press to form, hold the pressure for 10 minutes, and release the pressure to make a green sample. The green body sample was carbonized in argon, the heating rate was 6°C / min, the final carbonization temperature was 1050°C, and t...

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Abstract

The invention provides a preparation method of high-density ultrafine granular graphite for an ionization chamber, which comprises the following steps: crushing coal pitch, stirring with a first organic solvent at the temperature of 50-100 DEG C, extracting insoluble substances, crushing, and sufficiently stirring with a second organic solvent at the temperature of 50-100 DEG C to obtain a soluble substance solution; after the temperature of the ultrafine particle size aggregate carbon in the kneading machine reaches a preset temperature, adding the soluble substance solution as a binder into the kneading machine for liquid phase mixing, heating to a temperature higher than the boiling point of the second organic solvent, keeping the temperature constant, and evaporating the solvent to dryness to obtain a paste material; crushing the paste to obtain pressed powder; putting the pressed powder into a mold, pressing, molding, maintaining the pressure, and releasing the pressure to obtain a green body sample; carbonizing the green body sample in an inert atmosphere, heating to a first preset carbonization final temperature, and keeping the temperature to obtain a carbonized product; and carrying out impregnation densification treatment and pressure maintaining on the carbonized product, carrying out secondary carbonization after impregnation is completed, maintaining the final temperature of second preset carbonization, carrying out graphitization treatment and maintaining, cooling and discharging.

Description

technical field [0001] The invention relates to a technology for preparing high-density ultra-fine graphite for ionization chambers, and more particularly to a method for preparing high-density ultra-fine graphite for ionization chambers using a liquid-phase mixing process. Background technique [0002] High-density carbon / graphite material (density ≥ 1.82g / cm 3 , aggregate particle size ≤ 20μm) has low porosity, high specific strength, excellent thermal conductivity, high purity, good thermal shock resistance, self-lubricating inertness, good thermal stability in corrosive atmosphere, chemical corrosion to acid and alkali Strong stability and other characteristics, widely used in air ionization chamber, reactor moderator / reflector, reactor gamma radiation resistant interaxial sealing material, electric discharge machining, metal continuous casting, pulling single crystal silicon crucible, evaporator , Missile / rocket nozzles, space shuttle shaft seal materials and other civ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/532C04B35/622
CPCC04B35/532C04B35/522C04B35/622C04B2235/5436C04B2235/6562C04B2235/6567C04B2235/616C04B2235/77C04B2235/96C04B2235/9607
Inventor 程金星唐忠锋宋金亮王庆波于艾温伟伟连鹏飞吴友朋
Owner 中国人民解放军96901部队23分队
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