CN101905976B - Nano crystal magnesium oxide-carbon composite powder and preparation method thereof - Google Patents
Nano crystal magnesium oxide-carbon composite powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to nano crystal magnesium oxide-carbon composite powder and a preparation method thereof. The invention adopts the technical scheme that: magnesium carbonate, basic magnesium carbonate and metal magnesium powder are used as raw materials, and the method comprises the following steps of: mixing the magnesium carbonate and the metal magnesium powder in a molar ratio of 1:2 or mixing the basic magnesium carbonate and the metal magnesium powder in a molar ratio of 1:14 to form a mixed raw material, and adding 0 to 10 weight percent of metal nickel powder, 0 to 10 weight percent of metal iron powder and 0 to 10 weight percent of hydroxyl nickel powder of the mixed raw material to form a mixture; sealing the mixture and steel balls filled into a stainless steel ball grinding tank in a mass ratio of 1: (40-60), pumping vacuum to -0.1MPa and ball-milling the mixture for 2 to 50 hours on a planetary ball mill, or pumping vacuum to -0.1MPa and then introducing one of high-purity nitrogen, high-purity argon and CO2 gas into the mixture and ball-milling the mixture for 2 to 50 hours on a planetary ball mill to obtain the nano crystal magnesium oxide-carbon composite powder. The method has the advantages of simple process, easy industrialization and direct preparation; and the prepared nano crystal magnesium oxide-carbon composite powder has good interface combination and high dispersion degree.
Description
Technical field
The invention belongs to magnesium oxide-carbon composite powder technical field.Be specifically related to a kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.
Background technology
The carbon containing refractories such as magnesium carbon, aluminium carbon, magnalium carbon be last century the seventies add graphite on the basis of magnesite refractory and progressively grow up.Carbon (graphite) content in the tradition carbon containing refractory is generally 10～20%.Because graphite has higher thermal conductivity and not by characteristics such as slag infiltrations, resistance performance of slag corrosion and the antistrip performance of carbon containing refractory are greatly improved.Three during the last ten years, and carbon containing refractory is widely used in the positions such as steel-making converter, electric furnace, refining furnace furnace lining, ladle slag line and continuous-casting three-main-product.
In recent years, along with the development of Iron And Steel Industry and the progress of science and technology, smelting technology has also obtained fast development, and is also more and more higher to the service requirements of refractory materials.Reduce as far as possible or do not bring secondary pollution to molten steel such as the manufacturing technique requirent refractory materials of Clean Steel and ultra clean steel; Require the drop in temperature of molten steel can not be too large in the process of secondary refining, namely require furnace lining material to have low thermal conductivity.Obviously, traditional carbon containing refractory can not satisfy the service requirements of modern steel new process of production fully.In order to reduce energy consumption, avoid and reduce the refractory materials component molten steel is produced pollution, in the smelting process of Clean Steel and ultra clean steel, general requirement reduces the carbon content in the refractory materials as far as possible, uses Low carbon refractories.
Reduce the carbon content of carbon containing refractory, can reduce the thermal conductivity of material, but certainly will cause the decline of some performance of material: as, the thermal conductivity of material descends, and Young's modulus increases, and can cause the thermal shock resistance variation of material; In addition, after carbon content reduced, the wettability of slag and material strengthened, and performance and the anti-slag corrosion performance of material opposing slag penetration also can variation.Therefore, in the situation that graphite add-on decrease in the Low carbon refractories, how to guarantee that Low carbon refractories has good antistrip performance and anti-slag penetration, erosion performance is the important research direction of current Low carbon refractories research field.But partly introduce the nanoscale greying presoma that can promote the transformation of resin carbon graphite in matrix, also can effectively improve Low carbon refractories antioxidant property, antistrip performance and anti-slag penetration, erosion performance.The in recent years development of ultrafine powder technology of preparing also becomes possibility so that introduce nano-powder at ceramic matrix to its disperse enhancing.Adopt the means such as chemical Vapor deposition process, sol-gel method, hydrothermal method, microemulsion method can prepare particle diameter little of tens even the superfine powder of several nanometers; but these method complex manufacturing; be unfavorable for large-scale production; and nano-ceramic powder and nano-sized carbon particle can not prepare simultaneously, must join in the material after the mode blend by mechanically mixing again.Yet the high dispersing of the presoma of nanoscale in low carbon materials matrix is very crucial.This is because nano particle has strong volume effect, surface-interface effect etc.; add the effect of the surface tension etc. of intergranular Van der Waals force, electrostatic force and solvent; nano particle can produce serious reunion usually, and traditional mechanically mixing mode is difficult to destroy this aggregate structure.The existence of this aggregate structure can cause the inhomogeneous of material structure, and then affects the performance of material.
Summary of the invention
The present invention is intended to overcome the defective of prior art, and purpose provides the method that a kind of technique is simple, be easy to realize suitability for industrialized production, can directly prepare nano crystal magnesium oxide-carbon composite powder; With the prepared nano crystal magnesium oxide-carbon composite powder interface junction of the method get togather, have high degree of dispersion, crystal particle diameter is nano level, can avoid the excessive and dispersion problem of non-uniform of carbon in magnesium oxide powder of magnesium oxide crystal grain.
For achieving the above object, the technical solution used in the present invention is: adopting magnesiumcarbonate, magnesium basic carbonate and metal magnesium powder is raw material, be 1: 2 in molar ratio with magnesiumcarbonate and metal magnesium powder or be to mix at 1: 14 in molar ratio with magnesium basic carbonate and metal magnesium powder, form respectively mixing raw material, add the metal nickel powder of described mixing raw material 0～10wt%, the metal iron powder of 0～10wt% and the hydroxyl nickel powder of 0～10wt%, mix, form compound.
Or be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, and made nano crystal magnesium oxide-carbon composite powder;
Or be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, are filled with high pure nitrogen, high-purity argon gas and CO
2Then a kind of in the gas placed on the planetary ball mill ball milling 2～50 hours, makes nano crystal magnesium oxide-carbon composite powder.
In the technique scheme: magnesiumcarbonate is a kind of in magnesite, industrial carbonic acid magnesium, chemical pure magnesiumcarbonate, the analytical pure magnesiumcarbonate, and the particle diameter of magnesiumcarbonate is less than 100 orders; Magnesium basic carbonate is a kind of in industrial magnesium basic carbonate, chemical pure magnesium basic carbonate, the analytical pure magnesium basic carbonate, and the particle diameter of magnesium basic carbonate is less than 100 orders; The particle diameter of metal magnesium powder is less than 100 orders; The particle diameter of metal nickel powder, metal iron powder, hydroxyl nickel powder is all less than 100 orders; Steel ball is hardened steel ball, and the quality grating of steel ball is large ball: middle ball: bead=2: 4: 1; Large spherical diameter is 16mm, and middle spherical diameter is 10mm, and the small ball's diameter is 5mm.
Owing to adopting technique scheme, the present invention is take magnesiumcarbonate-metal magnesium powder and magnesium basic carbonate-metal magnesium powder as reaction system, adopt the method for mechanical alloying, the magnesiumcarbonate decomposition in situ reduction reaction of inducing by mechanical force under the normal temperature, directly preparation has the nano crystal magnesium oxide-carbon composite powder of high degree of dispersion.
This invention combines mechanical alloying and in-situ compositing at bitter earth nano intercrystalline original position generation strengthening phase carbon, compare with mechanically mixing doped graphite in magnesium oxide powder, 1. mechanical alloying and in-situ compositing combine, the direct nano crystal magnesium oxide-carbon composite powder of the standby high degree of dispersion of interlock system, technique is simple, be easy to realize suitability for industrialized production; 2. generated in-situ nanocrystalline graphite strengthening phase and bitter earth nano intercrystal boundary clean; 3. the distribution more tiny and between nanocrystalline magnesium oxide particle of the nanocrystalline graphite particle of strengthening phase is more even.
Therefore, the present invention have technique simple, be easy to realize industrialization, the characteristics that can directly prepare, prepared nano crystal magnesium oxide-carbon composite powder interface junction gets togather, has high degree of dispersion, crystal particle diameter is nano level, can avoid the excessive and dispersion problem of non-uniform of carbon in magnesium oxide powder of magnesium oxide crystal grain.
Description of drawings
Accompanying drawing 1～5 is the sign of a kind of nano crystal magnesium oxide-carbon composite powder of the present invention's preparation:
Fig. 1 is the X ray diffracting spectrum of this composite granule;
Fig. 2 is the X ray diffracting spectrum of this composite granule remaining powder of gained after persalt is processed and dried;
Fig. 3 be this composite granule through persalt process and oven dry after gained remaining powder the Raman spectrum analysis spectral line;
Fig. 4 and Fig. 5 are the high resolution transmitted electron image of this composite granule remaining powder of gained after persalt is processed and dried.
Embodiment
The invention will be further described below in conjunction with embodiment, is not the restriction to protection domain.
For avoiding repetition, the first grating unification of the physical and chemical parameter of the raw material that this embodiment is involved and steel ball is described below, and repeat no more among the embodiment: the particle diameter of magnesiumcarbonate, magnesium basic carbonate and metal magnesium powder is less than 100 orders; The particle diameter of metal nickel powder, metal iron powder, hydroxyl nickel powder is less than 100 orders; Steel ball is hardened steel ball, and the quality grating of steel ball is large ball: middle ball: bead=2: 4: 1; Large spherical diameter is 16mm, and middle spherical diameter is 10mm, and the small ball's diameter is 5mm.
Embodiment 1
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take magnesite and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with magnesite and metal magnesium powder, form mixing raw material.Be 1 with described mixing raw material and steel ball by the mass ratio of mixing raw material and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, then place on the planetary ball mill ball milling 2～50 hours, and made nano crystal magnesium oxide-carbon composite powder.
Embodiment 2
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial carbonic acid magnesium and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with industrial carbonic acid magnesium and metal magnesium powder, form mixing raw material.Be 1 with described mixing raw material and steel ball by the mass ratio of mixing raw material and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high pure nitrogen, placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 3
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with chemical pure magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder less than described mixing raw material 0.1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 4
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with analytical pure magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the metal iron powder less than described mixing raw material 0.1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, are filled with CO
2Then gas placed on the planetary ball mill ball milling 2～50 hours, makes nano crystal magnesium oxide-carbon composite powder.
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take magnesite and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with magnesite and metal magnesium powder, form mixing raw material, add the hydroxyl nickel powder less than described mixing raw material 0.1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 6
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take magnesite and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with magnesite and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 0.1～3wt%, the metal iron powder of 0.1～3wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 7
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial carbonic acid magnesium and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with industrial carbonic acid magnesium and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 0.1～3wt% and the hydroxyl nickel powder of 0.1～3wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, are filled with CO
2Then gas placed on the planetary ball mill ball milling 2～50 hours, makes nano crystal magnesium oxide-carbon composite powder.
Embodiment 8
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with chemical pure magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 0.1～3wt% and the hydroxyl nickel powder of 0.1～3wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high pure nitrogen, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 9
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with analytical pure magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 0.1～3wt% and the metal iron powder of 0.1～3wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Adopting magnesite and metal magnesium powder is raw material, be to mix at 1: 2 in molar ratio with magnesite and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 0.1～1wt%, the metal iron powder of 0.1～1wt% and the hydroxyl nickel powder of 0.1～1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high pure nitrogen, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 11
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take magnesite and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with magnesite and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 1～5wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 12
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial carbonic acid magnesium and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with industrial carbonic acid magnesium and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 1～5wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 13
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with chemical pure magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the hydroxyl nickel powder of described mixing raw material 1～5wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 14
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with analytical pure magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 3～8wt% and the metal iron powder of 3～8wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 15
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take magnesite and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with magnesite and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 3～8wt% and the hydroxyl nickel powder of 3～8wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 16
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial carbonic acid magnesium and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with industrial carbonic acid magnesium and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 3～8wt% and the hydroxyl nickel powder of 3～8wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 17
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with chemical pure magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 1～7wt%, the metal iron powder of 1～7wt% and the hydroxyl nickel powder of 1～7wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 18
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesiumcarbonate and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with magnesiumcarbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 5～10wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high pure nitrogen, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 19
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take magnesite and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with magnesite and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 5～10wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial carbonic acid magnesium and metal magnesium powder as raw material, be to mix at 1: 2 in molar ratio with industrial carbonic acid magnesium and metal magnesium powder, form mixing raw material, add the hydroxyl nickel powder of described mixing raw material 5～10wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, are filled with CO
2, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 21
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material.Be 1 with described mixing raw material and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, and made nano crystal magnesium oxide-carbon composite powder.
Embodiment 22
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material.Be 1 with described mixing raw material and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 23
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with chemical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder less than described mixing raw material 0.1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, then place on the planetary ball mill ball milling 2～50 hours, and made nano crystal magnesium oxide-carbon composite powder.
Embodiment 24
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with analytical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal iron powder less than described mixing raw material 0.1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, then place on the planetary ball mill ball milling 2～50 hours, and made nano crystal magnesium oxide-carbon composite powder.
Embodiment 25
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the hydroxyl nickel powder less than described mixing raw material 0.1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 26
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 0.1～3wt% and the hydroxyl nickel powder of 0.1～3wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 27
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with chemical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 0.1～3wt% and the hydroxyl nickel powder of 0.1～3wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 28
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with analytical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 0.1～3wt% and the metal iron powder of 0.1～3wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 29
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 0.1～1wt%, the metal iron powder of 0.1～1wt% and the hydroxyl nickel powder of 0.1～1wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with chemical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 1～7wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, are filled with CO
2Then gas placed on the planetary ball mill ball milling 2～50 hours, makes nano crystal magnesium oxide-carbon composite powder.
Embodiment 31
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 1～7wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 32
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the hydroxyl nickel powder of described mixing raw material 1～7wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high pure nitrogen, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 33
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with chemical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 3～8wt% and the metal iron powder of 3～8wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high pure nitrogen, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 34
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with analytical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 3～8wt% and the hydroxyl nickel powder of 3～8wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 35
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 3～8wt% and the hydroxyl nickel powder of 3～8wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, are filled with CO
2Then gas placed on the planetary ball mill ball milling 2～50 hours, makes nano crystal magnesium oxide-carbon composite powder.
Embodiment 36
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 1～7wt%, the metal iron powder of 1～7wt% and the hydroxyl nickel powder of 1～7wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, be evacuated to-0.1MPa, be filled with high-purity argon gas, then placed on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 37
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take chemical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with chemical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal nickel powder of described mixing raw material 5～10wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 38
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take analytical pure magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with analytical pure magnesium basic carbonate and metal magnesium powder, form mixing raw material, add the metal iron powder of described mixing raw material 5～10wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
Embodiment 39
A kind of nano crystal magnesium oxide-carbon composite powder and preparation method thereof.Take industrial magnesium basic carbonate and metal magnesium powder as raw material, be to mix at 1: 14 in molar ratio with industrial magnesium basic carbonate and metal magnesium powder, form respectively mixing raw material, add the hydroxyl nickel powder of described mixing raw material 5～10wt%, mix, form compound.Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder.
This embodiment is take magnesiumcarbonate-metal magnesium powder and magnesium basic carbonate-metal magnesium powder as reaction system, adopt the method for mechanical alloying, the magnesiumcarbonate decomposition in situ reduction reaction of inducing by mechanical force under the normal temperature, directly preparation has the nano crystal magnesium oxide-carbon composite powder of high degree of dispersion.Therefore have technique simple, be easy to realize industrialization, the characteristics that can directly prepare.
The prepared nano crystal magnesium oxide-carbon composite powder interface junction of this embodiment gets togather, and dispersity is high, and crystal particle diameter is nano level, can avoid the excessive and dispersion problem of non-uniform of carbon in magnesium oxide powder of magnesium oxide crystal grain.This embodiment combines mechanical alloying and in-situ compositing at bitter earth nano intercrystalline original position generation strengthening phase carbon.The accompanying drawing that characterizes take embodiment 4 prepared a kind of nano crystal magnesium oxide-carbon composite powders is as example:
Fig. 1 is the X ray diffracting spectrum of this composite granule, can find out magnesian existence; Fig. 2 is the X ray diffracting spectrum of this composite granule remaining powder of gained after persalt is processed and dried, and can see two main diffractive features peaks of carbon; Fig. 3 is the Raman spectrum analysis spectral line of this composite granule remaining powder of gained after persalt is processed and dried, and therefrom can find out two raman characteristic peaks of carbon, proves and contains carbon in the composite granule; Fig. 4 and Fig. 5 are the high resolution transmitted electron image of this composite granule remaining powder of gained after persalt is processed and dried.Therefrom can see carbon nano-crystal in the product composite granule, the existence of multiple-wall carbon nanotube and nano carbon microsphere.
Claims (7)
1. the preparation method of a nano crystal magnesium oxide-carbon composite powder, it is characterized in that: adopting magnesiumcarbonate, magnesium basic carbonate and metal magnesium powder is raw material, be 1: 2 in molar ratio with magnesiumcarbonate and metal magnesium powder or be to mix at 1: 14 in molar ratio with magnesium basic carbonate and metal magnesium powder, form respectively mixing raw material, add the metal nickel powder of described mixing raw material 0～10wt%, the metal iron powder of 0～10wt% and the hydroxyl nickel powder of 0～10wt%, mix, form compound;
Be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, place on the planetary ball mill ball milling 2～50 hours, make nano crystal magnesium oxide-carbon composite powder;
Or be 1 with described compound and steel ball by the mass ratio of compound and steel ball again: (40～60) are packed into and are sealed in the stainless steel jar mill, are evacuated to-0.1MPa, are filled with high pure nitrogen, high-purity argon gas and CO
2Then a kind of in the gas placed on the planetary ball mill ball milling 2～50 hours, makes nano crystal magnesium oxide-carbon composite powder.
2. the preparation method of nano crystal magnesium oxide-carbon composite powder according to claim 1 is characterized in that described magnesiumcarbonate is a kind of in magnesite, industrial carbonic acid magnesium, chemical pure magnesiumcarbonate, the analytical pure magnesiumcarbonate, and the particle diameter of magnesiumcarbonate is less than 100 orders.
3. the preparation method of nano crystal magnesium oxide-carbon composite powder according to claim 1, it is characterized in that described magnesium basic carbonate is a kind of in industrial magnesium basic carbonate, chemical pure magnesium basic carbonate, the analytical pure magnesium basic carbonate, the particle diameter of magnesium basic carbonate is less than 100 orders.
4. the preparation method of nano crystal magnesium oxide-carbon composite powder according to claim 1 is characterized in that the particle diameter of described metal magnesium powder is less than 100 orders.
5. the preparation method of nano crystal magnesium oxide-carbon composite powder according to claim 1 is characterized in that the particle diameter of described metal nickel powder, metal iron powder and hydroxyl nickel powder is all less than 100 orders.
6. the preparation method of nano crystal magnesium oxide-carbon composite powder according to claim 1 is characterized in that described steel ball is hardened steel ball, and the quality grating of steel ball is large ball: middle ball: bead=2: 4: 1; Large spherical diameter is 16mm, and middle spherical diameter is 10mm, and the small ball's diameter is 5mm.
7. the prepared nano crystal magnesium oxide-carbon composite powder of preparation method of each described nano crystal magnesium oxide-carbon composite powder according to claim 1～6.
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| CN101531345A (en) * | 2009-03-14 | 2009-09-16 | 骆天荣 | Method for producing nano powder by wet method for automatic liquid/solid separation |
| CN101778925A (en) * | 2007-08-20 | 2010-07-14 | 索尼公司 | Flame retardant agent, method for production of the flame retardant agent, resin composition, and method for production of the resin composition |
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| CN101778925A (en) * | 2007-08-20 | 2010-07-14 | 索尼公司 | Flame retardant agent, method for production of the flame retardant agent, resin composition, and method for production of the resin composition |
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