CN103708485B - Preparation method of scandium diboride - Google Patents
Preparation method of scandium diboride Download PDFInfo
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- CN103708485B CN103708485B CN201310731308.9A CN201310731308A CN103708485B CN 103708485 B CN103708485 B CN 103708485B CN 201310731308 A CN201310731308 A CN 201310731308A CN 103708485 B CN103708485 B CN 103708485B
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Abstract
The invention provides a preparation method of scandium diboride, which comprises the following steps: mixing a scandium-containing raw material and a boron-containing raw material, and sintering to obtain the scandium diboride, wherein the mol ratio of scandium in the scandium-containing raw material to boron in the boron-containing raw material is 1:(0.35-5). The purity of the scandium diboride prepared through the method provided by the invention can be up to 99%; and the preparation method is convenient, simple to operate and friendly to environment, produces less waste and fills up the blank of lacking a scandium diboride preparation method.
Description
Technical field
The present invention relates to two scandium boride technical fields, in particular to a kind of preparation method of two scandium borides.
Background technology
Two scandium boride (scb2) there is 2250 DEG C of high-melting-point, the microhardness under hot pressed samples room temperature up to 17.8gpa,
Resistivity is 7～15 μ ω cm, and thermoelectromotive force is 7.7 μ v/k, and density is 3.66g/cm3, because it has fusing point, hardness height,
Density is little, the low excellent materialization of resistivity and electric property, two scandium borides be considered as a kind of potential semi-conducting material,
Light-weight refractory and high-abrasive material.
Research now for two scandium borides focuses primarily upon the research to various aspects of performance, thunderous love soldier, Zhu Bo,
Extensively, Zhu Jun, Luan Cuixing, Yan Yonggang are at " first principle research (English) of elastic property under two scandium boride hardness and high pressure "
Local density approximation and the generalized gradient of density functional theory is used in (Sichuan University's journal (natural science edition) 06 phase in 2010)
Approximately descend plane-wave pseudo-potential, obtain elastic property under electronic structure, hardness and the high pressure of two scandium borides.From electronic structure
See, the chemical bond of two scandium borides is the mixing key with covalent, ion and metallic bond property.When there is no document pair in prior art
The preparation method of two scandium borides is inquired into.For studying properties and its potential use of two scandium borides further, need to grind
Study carefully and a kind of simple and easy to do, efficient energy-saving, eco-friendly two scandium boride preparation methoies.
Content of the invention
The present invention is intended to provide a kind of preparation method of two scandium borides, there is no two scandium boride preparation sides to solve prior art
The problem of method.
To achieve these goals, the invention provides a kind of preparation method of two scandium borides, including by raw material containing scandium and
Boracic raw material is mixed, and sintering obtains two scandium borides；The boron mol ratio of the scandium containing scandium raw material and boracic raw material be 1: 0.35～
5.
Further, containing scandium raw material scandium and boracic raw material boron mol ratio be 1: 2～4.
Further, carbon raw material is mixed with raw material containing scandium and boracic raw material.
Further, raw material containing scandium: the scandium containing scandium raw material: the boron of boracic raw material: the mol ratio of the carbon of carbon raw material is 1:
0.35～5: 0～3.5.
Further, the described scandium containing scandium raw material: the boron of boracic raw material: the mol ratio of the carbon of carbon raw material is 1: 2～4: 0
～2.5.
Further, raw material containing scandium is selected from Scia, scandium fluoride, Scium chloride (Sc4Cl12), Scium nitrate(Sc(NO3)3), acetic acid scandium and scandium carbonate or scandium is appointed
The group of one or any number of composition.
Further, raw material containing scandium is Scia.
Further, boracic raw material be selected from boron, boron oxide, boric acid, in boron carbide arbitrary or any number of composition group.
Further, boracic raw material is boron carbide.
Further, carbon raw material is selected from graphite, white carbon black or activated carbon is arbitrary or the group of any number of composition.
Further, sintering temperature is 1500～2000 DEG C.
Further, sintering temperature is 1500～1850 DEG C.
Further, sintering temperature is 1680～1750 DEG C.
Further, sintering time is 1～5 hour.
Further, sintering time is 1～3 hour.
Further, raw material is less than 270 microns for granularity.
Further, the step also including tabletting after mixed material step.
The method have technical effect that:
The method that the present invention provides only needs mixing, tabletting, sintering just to can get scb2Powder, this scb2Powder purity is maximum
Up to 99%.And this method processing step is easy, safe operation, environmental friendliness is suitable to industrial applicability.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.
Below with reference to embodiment, the present invention is further detailed explanation.
Brief description
The accompanying drawing constituting the part of the application is used for providing a further understanding of the present invention, the schematic reality of the present invention
Apply example and its illustrate, for explaining the present invention, not constituting inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is the two scandium boride powder diffraction analysis collection of illustrative plates that the preferred embodiment of the present invention is obtained.
Specific embodiment
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can phases
Mutually combine.To describe the present invention below in conjunction with embodiment in detail.
The boracic raw material of mix homogeneously and raw material containing scandium is made to react at high temperature using high-temperature sintering process in the present invention,
Obtain highly purified two scandium borides.
The method that the present invention provides passes through to mix raw material containing scandium and boracic raw material, and sintering directly obtains two scandium borides.Containing scandium
When sintering after raw material and the mixing of boracic raw material, primary response equation is: sc+b → scb2.Now raw material containing scandium can be arbitrarily normal
With material containing scandium, boracic raw material can be the conventional high temperature sintering material of any boracic.With selected raw material containing scandium and boracic raw material
Difference, the reaction being occurred in addition to primary response, also can according in raw material add other elements occur at high temperature accordingly
Reaction.But it is conventionally used for raw material containing scandium and the boracic raw material of high temperature sintering, other atoms contained, after high temperature sintering, no
This reaction can be impacted, after oversintering, remain to two scandium borides are obtained.Obviously contained herein other elements are in height
When can volatilize in a gaseous form under temperature, gained two scandium boride purity can be improved.
When raw material containing scandium is Scia, boracic raw material can for arbitrarily conventional containing boron substance for example boron, boron oxide, boric acid,
The group of arbitrary or any number of composition in boron carbide, now primary response equation be: sc2o3+b→scb2+bo↑.By this reaction side
Formula, preferably raw material containing scandium are Scia is boron simple substance with boracic raw material, and now the two directly reacts, and is producing two boronations
Form oxidation boron vapour while scandium, only exist two scandium boride solids in products therefrom, thus can guarantee that gained two scandium boride
Purity.
In reaction raw material containing scandium be reduced into free scandium atom then with the boron atom restoring from boracic raw material, sintering
At a temperature of combined with covalent bond, ionic bond and three kinds of modes of metallic bond and generate two scandium borides.
Obviously raw material containing scandium herein can be for arbitrarily containing the material of scandium.Preferably raw material containing scandium be Scia, scandium fluoride,
Scium chloride (Sc4Cl12), Scium nitrate(Sc(NO3)3), acetic acid scandium and scandium carbonate or scandium is arbitrary or the group of any number of composition.The conventional material containing scandium is through often
After rule method process forms Scia, could be used in the method for present invention offer, conventional treatment method herein, including but not
It is limited to the conventional treatment means such as co-precipitation and obtain Scia.Scia is made to participate in two boronations by the method that the present invention provides again afterwards
The generation of scandium.Certainly the raw material containing scandium having originally just directly oxidized can participate in reaction under the conditions of high temperature sintering, now should
Material does not need individual processing to add in reaction after becoming Scia, such as Scium nitrate(Sc(NO3)3), scandium carbonate etc..Coprecipitated in the present invention
Shallow lake method can be the coprecipitation mentioned in the coprecipitation such as cn200910206271 of arbitrary conventional process rare earth element.Containing scandium
Raw material is more preferably Scia, can energy saving, reduce preprocessor.
Obviously boracic raw material herein can be the material of any boracic, and preferred boracic raw material is boron, boron oxide, boron
Acid, in boron carbide arbitrary or any number of composition group.More preferably boron carbide.
In course of reaction, the mixed proportion of raw material containing scandium and boracic raw material is the scandium containing scandium raw material and described boracic raw material
Boron mol ratio is 1: 0.35～5 mixing.If do not mixed in this ratio, in course of reaction, the ratio of scandium element and boron element cannot
Meet 1: 2 atomic ratio requirement, products therefrom just cannot ensure to only generate two scandium borides, can there are many unknown by-products
Thing, thus affect the purity of product.Preferably raw material containing scandium and boracic raw material press the mol ratio of sc and b and are mixed for 1: 2～4.Press
This ratio is mixed to prepare two scandium boride purity and reaches as high as more than 99%.
Obviously carbon raw material can also be added in the feed, carbon raw material can provide catalytic reducer carbon list for reaction
Matter, during the course of the reaction, the boron in boracic raw material is reduced to boron simple substance by carbon at high temperature first, and with boracic raw material in its
He combines so as to be easy to leave from product material.Scandium in raw material containing scandium is restored by carbon again afterwards, and will contain scandium raw material
In other materials take away product, the scandium simple substance being formed during the course of the reaction and boron simple substance, surface reaction activity is than higher than direct
Scandium simple substance is used for reacting with boron simple substance.The combination speed of scandium and boron can be improved so as to generation two scandium boride of rapid, high volume.Carbon
Addition form be not limited to individually add carbon raw material it is also possible to by adding the boracic of the raw material containing scandium of carbon containing or carbon containing former
Material, such as boron carbide.As long as the carbon being added is easy to participate in reaction under the conditions of high temperature sintering, can be by other materials in raw material with gas
Body form takes away reaction system,.
When raw material containing scandium is Scia, and boracic raw material is boron carbide, by sc2o3+b4c→scb2+co↑+bo↑+co2↑+
b2o2↑ react, except other materials of two scandium borides all leave in gaseous form in products therefrom, thus can obtain pure
Two scandium borides.When raw material containing scandium is Scia, boracic raw material is boron carbide, when carbon raw material is carbon simple substance, by sc2o3+b4c+c
→scb2+ co ↑ react, due to only generating CO (carbon monoxide converter) gas, thus gained two scandium boride purity is protected.
Carbon raw material preferably comprises graphite, white carbon black or activated carbon is arbitrary or the group of any number of composition.These materials are equal
For the carbon simple substance of powder, can directly play the effect of catalysis reduction.The addition of carbon raw material is more than zero.Raw material containing scandium
Scandium: the boron of boracic raw material: the carbon of carbon raw material in molar ratio be 1: 0.35～5: 0～3.5 mixing, carbon raw material carbon massage
You are less than 3.5 additions than more than zero.Carbon raw material is added to can guarantee that carbon raw material gives full play to catalysis and goes back original work in this ratio
Wasted moreover it is possible to accelerate the carrying out of reaction with avoid raw material again, improve the purity of two scandium borides.Preferably, raw material raw material containing scandium,
The mol ratio that boracic raw material, carbon raw material press sc, b and c is 1: 2～4: 0～2.5 mixing.In obtained two boron of this ratio mixing
Change scandium purity up to more than 99%.
In preparation process, sintering temperature is 1350～2000 DEG C, can guarantee that being smoothed out of reaction by this temperature, if warm
Spend low, then reaction cannot occur, and will not generate two scandium boron.The waste of the energy if temperature is too high, can be caused, increase anti-
The generation of the side reaction during answering, reduces the purity of resulting material.Although being reacted by this temperature range and being can guarantee that reaction
Generation but gained two scandium boride purity is relatively low.It has been generally acknowledged that the higher two scandium boride purity of sintering temperature should be higher, but actual
But be two scandium borides in the products therefrom when sintering temperature is the closer to 1500 DEG C purity higher.Further preferred sintering temperature
For 1500～1850 DEG C, it is improved by this temperature sintering gained two scandium boride purity.Optimum sintering temperature is 1680～
1750℃.Now the purity of two scandium borides is up to 99%.
Sintering time can carry out appropriateness test according to standard empirical and obtain a rational scope.This is because during sintering
Between length can affect react carry out degree, when temperature is increased to preset range, reaction start occur, but reaction start after
Shortly lower the temperature, then reaction can not fully be carried out, and can remain the product mixing in a large number with raw material, and resulting material separating-purifying is stranded
Difficult.And it is long to work as sintering time, can waste the energy.Thus preferably, sintering time is 1～5 hour.Both sinter by this time
The energy will not be wasted and can guarantee that raw material fully reacts again.Preferably sintering time is 1～3 hour, and now raw material reaction is the most abundant,
Gained two scandium boride purity is up to 99%.
Two scandium borides equally can be prepared when raw material is for block.Due to being sintered to solid state reaction, raw material granularity
Size all has an impact to the purity of resulting material and the extent of reaction.When raw material particle size is less than 270 microns, more equal after powder mixing
Even, contact with each other fully after the little mixing of material particular diameter, contact area is big, is conducive to being swift in response, is sufficiently carried out, thus improving
The purity of product.When the particle diameter of raw material thing is less than 270 microns, the purity of gained two scandium boride is up to 99%.Due to raw material
Particle diameter all has an impact to the carrying out of reaction and the purity of final product.Preferably mixed material is carried out compressing tablet process, to add
Contact area between each component powders and contact depth in big raw material, the carrying out that intensification is reacted, thus improve the carrying out of reaction.Warp
Re-sinter after crossing compressing tablet process, the purity of gained two scandium boride is up to 99%.Tabletting is carried out according to a conventional method.Mixed material step
Can mix for hand operated mixing, mechanical agitation mixes, mediates, sieve the various conventional mixed medias such as mixing or ball milling mixing.For
Promote the mixing uniformity of raw material, preferably use ball milling mixing.Raw material mixing can be promoted to pass through using ball milling mixing again
The particle diameter of raw material is reduced by the grinding of ball-milling medium further, and each feed particles can also be extruded in mechanical milling process so as to
It is adjacent to each other or even embedded, be conducive to the generation of subsequent reactions.In order to prevent the introducing of impurity element, the liner of ball mill is preferred
Corundum.
Sintering is to carry out in reaction crucible, and crucible material can select the exotic material such as graphite, tantalum, molybdenum, these things
Matter not with reactant reaction.Sintering heating is carried out using vacuum resistance furnace or carbon shirt-circuiting furnace, presses 5～20 DEG C/minute in sintering process
Clock is heated up.After oversintering, gained two scandium boride is easily broken, obtains powder after simple crushing.
Embodiment
In following examples, each material used and instrument are commercially available.
In following examples, raw material containing scandium used is Scia, scandium fluoride, Scium chloride (Sc4Cl12), Scium nitrate(Sc(NO3)3), acetic acid scandium and scandium carbonate
Or scandium arbitrary when, need if necessary first to carry out co-precipitation by the method in cn200910206271 to be processed as putting into again after Scia to make
With weighing raw materials used during raw material is Scia, scandium fluoride, Scium chloride (Sc4Cl12), Scium nitrate(Sc(NO3)3), acetic acid scandium and scandium carbonate or scandium is arbitrary.
Embodiment 1
With Scia (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 270 microns, by sc2o3∶b4C: c mol ratio is 1: 1: 2 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 99%.
Embodiment 2
With Scia (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is less than carbon dust (analysis is pure)
270 microns, by sc2o3∶b4C: c mol ratio is 1: 1.2: 1.5 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction earthenware
In crucible.It is subsequently placed in resistance furnace, under vacuum, rises to 1700 DEG C with the heating rate of 5～20 DEG C/min, insulation 3 is little
When, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 99%.
Embodiment 3
With Scia (more than 99%), boron carbide (more than 99%), activated carbon powder (analysis is pure) as raw material, the granularity of raw material
Less than 270 microns, by sc2o3∶b4C: c mol ratio is 1: 2: 2.5 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction
In crucible.It is subsequently placed in resistance furnace, under vacuum, rises to 1750 DEG C with the heating rate of 5～20 DEG C/min, be incubated 4
Hour, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 99%.
Embodiment 4
With Scia (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 270 microns, by sc2o3∶b4C: c mol ratio is 1: 1.5: 0.001 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads anti-
Answer in crucible.It is subsequently placed in resistance furnace, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, insulation
2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 99%.
Embodiment 5
With scandium fluoride (more than 99%), boron (more than 99%), as raw material, the granularity of raw material is less than graphite powder (analysis is pure)
340 microns, by raw material containing scandium: boracic raw material: the mol ratio of carbon raw material is 1: 0.65: 2 dispensing, grinds after being sufficiently mixed uniformly
Tabletting, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, risen to the heating rate of 5～20 DEG C/min
1500 DEG C, it is incubated hour, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than
82%.
Embodiment 6
With scandium fluoride (more than 99%), boron (more than 99%), as raw material, the granularity of raw material is less than graphite powder (analysis is pure)
500 microns, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1: 5: 3.5 dispensing, grinds fully mixed
Tabletting after closing uniformly, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with the intensification of 5～20 DEG C/min
Speed rises to 2000 DEG C, is incubated 5 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder,
Purity is more than 50%.
Embodiment 7
With scandium fluoride (more than 99%), boron (more than 99%), graphite powder (analysis is pure) as raw material, the granularity of raw material is less than 70
Micron, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1: 2: 2.5 dispensing, grinding is sufficiently mixed
Tabletting after uniformly, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with the intensification speed of 5～20 DEG C/min
Rate rises to 1850 DEG C, is incubated 3 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder is pure
Degree is more than 70%.
Embodiment 8
With Scium nitrate(Sc(NO3)3) (more than 99%), boric acid (more than 99%), as raw material, the granularity of raw material is less than graphite powder (analysis is pure)
300 microns, by raw material containing scandium: boracic raw material: the mol ratio of carbon raw material is 1: 0.74: 3.2 dispensing, grinds and is sufficiently mixed uniformly
Tabletting afterwards, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with the heating rate liter of 5～20 DEG C/min
To 1750 DEG C, it is incubated 1 hour, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is big
In 30%.
Embodiment 9
With Scium nitrate(Sc(NO3)3) (more than 99%), boric acid (more than 99%), graphite powder (analysis is pure) as raw material, by raw material containing scandium: contain
Boron raw material: in carbon raw material, the mol ratio of sc, b and c is 1: 2: 0.001 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads anti-
Answer in crucible.It is subsequently placed in resistance furnace, under vacuum, rise to 1680 DEG C with the heating rate of 5～20 DEG C/min, insulation
2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 50%.
Embodiment 10
With Scium nitrate(Sc(NO3)3) (more than 99%), boric acid (more than 99%), as raw material, the granularity of raw material is less than graphite powder (analysis is pure)
400 microns, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1: 3: 1.4 dispensing, grinds fully mixed
Tabletting after closing uniformly, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with the intensification of 5～20 DEG C/min
Speed rises to 1760 DEG C, is incubated 4 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder,
Purity is more than 65%.
Embodiment 11
With acetic acid scandium (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 700 microns, by raw material containing scandium: boracic raw material: in carbon raw material, sc, b and c mol ratio is 1:2.7:0.4 dispensing, grinds fully
Tabletting after mix homogeneously, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with the liter of 5～20 DEG C/min
Warm speed rises to 1510 DEG C, is incubated 2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder
End, purity is more than 70%.
Embodiment 12
With acetic acid scandium (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 220 microns, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1:3.2:2 dispensing, grinds fully
Tabletting after mix homogeneously, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with the liter of 5～20 DEG C/min
Warm speed rises to 1630 DEG C, is incubated 2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder
End, purity is more than 65%.
Embodiment 13
With acetic acid scandium (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 210 microns, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1:0.9:3.4 dispensing, grinding is filled
Divide tabletting after mix homogeneously, load in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with 5～20 DEG C/min's
Heating rate rises to 1750 DEG C, is incubated 2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder
End, purity is more than 54%.
Embodiment 14
With scandium carbonate (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 100 microns, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1:1.2:2.3 dispensing, grinding is filled
Divide tabletting after mix homogeneously, load in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with 5～20 DEG C/min's
Heating rate rises to 1490 DEG C, is incubated 2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder
End, purity is more than 52%.
Embodiment 15
With scandium carbonate (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 110 microns, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1:2:0.04 dispensing, grinding is filled
Divide tabletting after mix homogeneously, load in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with 5～20 DEG C/min's
Heating rate rises to 1530 DEG C, is incubated 2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder
End, purity is more than 55%
Embodiment 16
With scandium carbonate (more than 99%), boron carbide (more than 99%), as raw material, the granularity of raw material is little for graphite powder (analysis is pure)
In 270 microns, by raw material containing scandium: boracic raw material: in carbon raw material, the mol ratio of sc, b and c is 1:3:0.3 dispensing, grinds fully
Tabletting after mix homogeneously, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with the liter of 5～20 DEG C/min
Warm speed rises to 1720 DEG C, is incubated 2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder
End, purity is more than 60%.
Embodiment 17
With scandium (more than 99%), boron (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by scandium: boron mole
Ratio for 1:1 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads in reaction crucible.It is subsequently placed in resistance furnace, in vacuum condition
Under, rise to 1780 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, the scb obtaining2Ground
Sieve just finished product scb2Powder, purity is more than 60%.
Embodiment 18
With scandium (more than 99%), boron (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by scandium: boron mole
Ratio for 1:2 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads in reaction crucible.It is subsequently placed in resistance furnace, in vacuum condition
Under, rise to 1720 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, the scb obtaining2Ground
Sieve just finished product scb2Powder, purity is more than 90%.
Embodiment 19
With scandium (more than 99%), boron (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by scandium: boron mole
Ratio for 1:2.2 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads in reaction crucible.It is subsequently placed in resistance furnace, in vacuum bar
Under part, rise to 1730 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, the scb obtaining2Through grinding
Honed sieve just finished product scb2Powder, purity is more than 95%.
Embodiment 20
With Scia (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
sc2o3: b4The mol ratio of c is 1:0.7 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads in reaction crucible.It is subsequently placed in electricity
In resistance stove, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down,
The scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 65%.
Embodiment 21
With Scia (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, presses
sc2o3: b4The mol ratio of c is 1:2.5 dispensing, loads in reaction crucible.It is subsequently placed in resistance furnace, under vacuum, with 5
The heating rate of～20 DEG C/min rises to 1600 DEG C, is incubated 2 hours, then cooling down, the scb obtaining2Ground sieve just
Finished product scb2Powder, purity is more than 75%.
Embodiment 22
With Scia (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, presses
sc2o3: b4The mol ratio of c is 1:1 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads in reaction crucible.It is subsequently placed in resistance
In stove, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, obtain
The scb arriving2The ground just finished product scb that sieves2Powder, purity is more than 82.5%.
Embodiment 23
With Scia (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, presses
sc2o3: b4The mol ratio of c is 1:1.25 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads in reaction crucible.It is subsequently placed in electricity
In resistance stove, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down,
The scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 90%.
Embodiment 24
With Scia (more than 99%), boric acid (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by sc2o3:
h3bo3Mol ratio be 1:2 dispensing, grind be sufficiently mixed uniformly after tabletting, load reaction crucible in.It is subsequently placed in resistance furnace,
Under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, obtain
scb2The ground just finished product scb that sieves2Powder, purity is more than 50%.
Embodiment 25
With Scia (more than 99%), boron oxide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, presses
sc2o3: h3bo3Mol ratio be 1:4 dispensing, grind be sufficiently mixed uniformly after tabletting, load reaction crucible in.It is subsequently placed in electricity
In resistance stove, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down,
The scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 80%.
Embodiment 26
With Scia (more than 99%), boron (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by sc2o3:
h3bo3Mol ratio be 1:5 dispensing, grind be sufficiently mixed uniformly after tabletting, load reaction crucible in.It is subsequently placed in resistance furnace,
Under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, obtain
scb2The ground just finished product scb that sieves2Powder, purity is more than 85%.
Embodiment 27
With scandium fluoride (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:1 dispensing, loads in reaction crucible.It is subsequently placed in resistance furnace, in vacuum
Under the conditions of, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, the scb obtaining2Warp
Grinding is sieved just finished product scb2Powder, purity is more than 50%.
Embodiment 28
With scandium fluoride (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:1.5 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 65%.
Embodiment 29
With scandium fluoride (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:2 dispensing, loads in reaction crucible.It is subsequently placed in resistance furnace, in vacuum
Under the conditions of, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, the scb obtaining2Warp
Grinding is sieved just finished product scb2Powder, purity is more than 80%.
Embodiment 30
With Scium chloride (Sc4Cl12) (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:1.4 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 60%.
Embodiment 31
With Scium chloride (Sc4Cl12) (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:2.7 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 80%.
Embodiment 32
With Scium chloride (Sc4Cl12) (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:3.4 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 72%.
Embodiment 33
With Scium nitrate(Sc(NO3)3) (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:3.2 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 70%.
Embodiment 34
With Scium nitrate(Sc(NO3)3) (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:2.7 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 80%.
Embodiment 35
With Scium nitrate(Sc(NO3)3) (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:1.4 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 55%.
Embodiment 36
With acetic acid scandium (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:1.8 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 60%.
Embodiment 37
With acetic acid scandium (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:1.4 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 50%.
Embodiment 38
With acetic acid scandium (more than 99%), boron carbide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material sc and b is 1:1.7 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction crucible
In.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours,
Then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 56%.
Embodiment 39
With Scia (more than 99%), boron oxide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, presses
sc2o3: b2o3Mol ratio be 1:1.6 dispensing, grind be sufficiently mixed uniformly after tabletting, load reaction crucible in.It is subsequently placed in electricity
In resistance stove, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down,
The scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 40%.
Embodiment 40
With Scia (more than 99%), boron oxide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, presses
sc2o3: b2o3Mol ratio be 1:2 dispensing, grind be sufficiently mixed uniformly after tabletting, load reaction crucible in.It is subsequently placed in resistance
In stove, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then cooling down, obtain
The scb arriving2The ground just finished product scb that sieves2Powder, purity is more than 70%.
Embodiment 41
With Scia (more than 99%), boron oxide (more than 99%) as raw material, the granularity of raw material is less than 270 microns, by containing
Scandium raw material: the mol ratio of boracic raw material is 1:2.5 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads in reaction crucible.Then
It is placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2 hours, then drop
Temperature cooling, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 80%.
Embodiment 42
With Scia (more than 99%), boron oxide (more than 99%), activated carbon (more than 99%) as raw material, the granularity of raw material
Less than 270 microns, by sc2o3: b2o3: the mol ratio of c is 1:2:1 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads reaction
In crucible.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, be incubated 2
Hour, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 70%.
Embodiment 43
With Scia (more than 99%), boron oxide (more than 99%), activated carbon (more than 99%) as raw material, the granularity of raw material
Less than 270 microns, by sc2o3: b2o3: the mol ratio of c is 1:2.2:1 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads anti-
Answer in crucible.It is subsequently placed in resistance furnace, under vacuum, rise to 1600 DEG C with the heating rate of 5～20 DEG C/min, insulation
2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 75%.
Embodiment 44
With Scia (more than 99%), boron oxide (more than 99%), activated carbon (more than 99%) as raw material, the granularity of raw material
Less than 270 microns, by sc2o3: b2o3: the mol ratio of c is 1:2.2:1.5 dispensing, grinds and is sufficiently mixed tabletting after uniformly, loads
In reaction crucible.It is subsequently placed in resistance furnace, under vacuum, rises to 1600 DEG C with the heating rate of 5～20 DEG C/min, protect
Temperature 2 hours, then cooling down, the scb obtaining2The ground just finished product scb that sieves2Powder, purity is more than 90%.
By embodiment 1～4 gained scb2Powder measures powder diffraction analysis collection of illustrative plates as shown in figure 1, two scandium boride samples are bent
Line is understood with two scandium boride standard curve contrasts below this curve, the peak (001) (100) on two scandium boride sample curves
(101) (002) (110) (102) (111) (200) (201) all can be corresponding with the peak on two scandium boride standard curves.Gained is described
Product is the higher scb of purity2Powder.
Embodiment 5～44 products therefrom measures powder diffraction analysis collection of illustrative plates, finds all to can detect that two boron in products therefrom
Change scandium, in product, two scandium boride contents are minimum also can reach 30%, simple and effective being obtained of method energy that the present invention provides is described
Two high scandium borides of purity, are that the industrial applicability of two scandium borides is ready.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for those skilled in the art
For member, the present invention can have various modifications and variations.All any modifications within the spirit and principles in the present invention, made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of two scandium borides is it is characterised in that include entering carbon raw material with raw material containing scandium and boracic raw material
Row mixing, sintering obtains described two scandium borides；The described scandium containing scandium raw material: the boron of boracic raw material: the carbon of carbon raw material mole
Than for 1:2～4:0～2.5；Described raw material granularity is less than 270 microns；Described sintering temperature is 1680～1750 DEG C；Described sintering
Time is 1～3 hour；The step that described preparation method also includes tabletting after described mixed material step.
2. preparation method according to claim 1 is it is characterised in that described raw material containing scandium is selected from Scia, scandium fluoride, chlorine
Change scandium, Scium nitrate(Sc(NO3)3), acetic acid scandium and scandium carbonate or scandium is arbitrary or the group of any number of composition.
3. preparation method according to claim 2 is it is characterised in that described raw material containing scandium is Scia.
4. preparation method according to claim 1 it is characterised in that described boracic raw material be selected from boron, boron oxide, boric acid,
The group of arbitrary or any number of composition in boron carbide.
5. preparation method according to claim 4 is it is characterised in that described boracic raw material is boron carbide.
6. preparation method according to claim 1 is it is characterised in that described carbon raw material is selected from graphite, white carbon black or activity
Charcoal is arbitrary or the group of any number of composition.
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| CN114230372B (en) * | 2021-12-22 | 2022-11-22 | 连云港太阳光石英陶瓷有限公司 | Corrosion-resistant high-strength ceramic roller and preparation method thereof |
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| CN102584242A (en) * | 2012-02-28 | 2012-07-18 | 吉林大学 | High-temperature high-pressure preparation method for titanium diboride |
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