CN103708485A - Preparation method of scandium diboride - Google Patents
Preparation method of scandium diboride Download PDFInfo
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- CN103708485A CN103708485A CN201310731308.9A CN201310731308A CN103708485A CN 103708485 A CN103708485 A CN 103708485A CN 201310731308 A CN201310731308 A CN 201310731308A CN 103708485 A CN103708485 A CN 103708485A
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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 (ScB
2) thering is the high-melting-point of 2250 ℃, the microhardness under hot pressed samples room temperature can reach 17.8Gpa, and resistivity is 7～15 μ Ω cm, and thermoelectromotive force is 7.7 μ V/K, and density is 3.66g/cm
3, because it has fusing point, hardness is high, density is little, materialization and electric property that the low grade of resistivity is excellent, and two scandium borides are considered to a kind of potential semiconductor material, light-weight refractory and high-abrasive material.
Research for two scandium borides now mainly concentrates on the research to various aspects of performance, thunderous love soldier, Zhu Bo, Zhang Guang, Zhu Jun, Luan Cuixing, local density approximation and generalized gradient by density functional theory in first principle research (English) > > (Sichuan University's journal (natural science edition) 06 phase in 2010) of Yan Yonggang elastic property under < < bis-scandium boride hardness and high pressure are similar to lower pseudo potential plane wave, obtained the electronic structure of two scandium borides, elastic property under hardness and high pressure.From electronic structure, the chemical bond of two scandium borides is the mixing keys with covalency, ion and metallic bond character.In prior art, do not have document to inquire into the preparation method of two scandium borides.For further properties and the potential use thereof of research two scandium borides, need to work out a kind of simple and easy to do, efficient energy-saving, eco-friendly two scandium boride preparation methods.
Summary of the invention
The present invention aims to provide a kind of preparation method of two scandium borides, there is no two scandium boride preparation methods' problem to solve prior art.
To achieve these goals, the invention provides a kind of preparation method of two scandium borides, comprise and will mix containing scandium raw material and boracic raw material, sintering obtains two scandium borides; Containing the scandium of scandium raw material and the boron mol ratio of boracic raw material, be 1: 0.35～5.
Further, containing scandium raw material scandium and the mol ratio of the boron of boracic raw material be 1: 2～4.
Further, by carbon raw material with containing scandium raw material and boracic raw material, mix.
Further, containing scandium raw material: the scandium that contains 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, containing scandium raw material, be selected from Scium trioxide, scandium fluoride, Scium trichloride, Scium trinitrate, acetic acid scandium and scandium carbonate or scandium is arbitrary or the group of any number of compositions.
Further, containing scandium raw material, be Scium trioxide.
Further, boracic raw material is selected from the group of arbitrary in boron, boron oxide, boric acid, norbide or any number of compositions.
Further, boracic raw material is norbide.
Further, carbon raw material is selected from the group of the arbitrary or any number of compositions of graphite, carbon black or gac.
Further, sintering temperature is 1500～2000 ℃.
Further, sintering temperature is 1500～1850 ℃.
Further, sintering temperature is 1680～1750 ℃.
Further, sintering time is 1～5 hour.
Further, sintering time is 1～3 hour.
Further, raw material is that granularity is less than 270 microns.
Further, the step that also comprises compressing tablet after mixing raw material step.
Technique effect of the present invention is:
Method provided by the invention only needs mixing, compressing tablet, sintering just can obtain ScB
2powder, this ScB
2powder purity maximum can reach 99%.And this method processing step is easy, operational safety, environmental friendliness is suitable for industrial applicability.
Except object described above, feature and advantage, the present invention also has other object, feature and advantage.Below with reference to embodiment, the present invention is further detailed explanation.
Accompanying drawing explanation
The accompanying drawing that forms the application's a part is used to provide a further understanding of the present invention, and schematic description and description of the present invention is used for explaining the present invention, does not form 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 makes.
Embodiment
It should be noted that, in the situation that not conflicting, embodiment and the feature in embodiment in the application can combine mutually.Below in conjunction with embodiment, describe the present invention in detail.
In the present invention, adopt high-temperature sintering process make the boracic raw material mixing and at high temperature react containing scandium raw material, obtain highly purified two scandium borides.
Method provided by the invention contains scandium raw material and boracic raw material by mixing, and sintering directly obtains two scandium borides.During containing scandium raw material and the rear sintering of boracic raw material mixing, main reaction equation is: Sc+B → ScB
2.Now can be for conventional containing scandium material arbitrarily containing scandium raw material, boracic raw material can be the conventional high temperature sintering material of any boracic.With the selected difference containing scandium raw material and boracic raw material, except main reaction, also can at high temperature there is corresponding reaction according to other elements that add in raw material in the reaction occurring.But conventional for high temperature sintering containing scandium raw material and boracic raw material, contained other atoms, after high temperature sintering, can, to the impacting of this reaction, after oversintering, still can not make two scandium borides.When obviously contained other elements at high temperature can volatilize with gaseous form, can improve gained two scandium boride purity herein.
When being Scium trioxide containing scandium raw material, boracic raw material can be for the conventional boron substance that contains is as the group of arbitrary in boron, boron oxide, boric acid, norbide or any number of compositions arbitrarily, and now main reaction equation is: Sc
2o
3+ B → ScB
2+ BO ↑.By this reaction equation, containing scandium raw material, be preferably that Scium trioxide and boracic raw material are boron simple substance, now the two directly reacts, and when producing two scandium borides, forms boron oxide steam, in products therefrom, only there are two scandium boride solids, thereby can guarantee the purity of gained two scandium borides.
In reaction containing scandium raw material be reduced into free scandium atom then with the boron atom restoring from boracic raw material, under sintering temperature with covalent linkage, ionic linkage and three kinds of modes of metallic bond in conjunction with generating two scandium borides.
The obvious scandium raw material that contains herein can be to contain arbitrarily the material of scandium.Preferred is Scium trioxide, scandium fluoride, Scium trichloride, Scium trinitrate, acetic acid scandium and scandium carbonate or scandium is arbitrary or the group of any number of compositions containing scandium raw material.The conventional material containing scandium is processed and is formed after Scium trioxide through ordinary method, all can be used for method provided by the invention, and conventional treatment method herein, includes but not limited to that the conventional processing means such as co-precipitation obtain Scium trioxide.By method provided by the invention, make Scium trioxide participate in the generation of two scandium borides more afterwards.What certainly have originally just can react containing scandium raw material under high temperature sintering condition in direct oxidized participation, and now this material does not add in reaction after not needing individual curing to become Scium trioxide again, and as Scium trinitrate, scandium carbonate etc. all can.In the present invention, coprecipitation method can be for the coprecipitation method of arbitrary conventional processing rare earth element be as the coprecipitation method of mentioning in CN200910206271.Containing scandium raw material Scium trioxide more preferably, can save energy, reduce preprocessor.
Obvious boracic raw material herein can be the material of any boracic, and preferred boracic raw material is the group of arbitrary in boron, boron oxide, boric acid, norbide or any number of compositions.Norbide more preferably.
Blending ratio containing scandium raw material and boracic raw material in reaction process is 1: 0.35～5 mixing for containing the scandium of scandium raw material and the boron mol ratio of described boracic raw material.If mixed not according to this ratio, in reaction process, the ratio of scandium element and boron cannot meet the atomic ratio requirement of 1: 2, and products therefrom just cannot guarantee only to generate two scandium borides, can have the by product of many unknowns, thereby affects the purity of product.Preferred is 1: 2～4 mixing containing scandium raw material and boracic raw material by the mol ratio of Sc and B.In this ratio mixing, making two scandium boride purity reaches as high as more than 99%.
Obviously in raw material, can also add carbon raw material, carbon raw material can provide catalytic reducer carbon simple substance for reaction, and in reaction process, first carbon be at high temperature reduced to boron simple substance by the boron in boracic raw material, and other materials in boracic raw material are combined, make it be easy to leave from product.Carbon restores the scandium containing in scandium raw material again afterwards, and other materials containing in scandium raw material are taken away to product, the scandium simple substance forming in reaction process and boron simple substance, and surface reaction activity ratio is higher than directly scandium simple substance and boron simple substance being used for reacting.Can improve the combination speed of scandium and boron, make generation two scandium borides of its rapid, high volume.The form that adds of carbon is not limited to add separately carbon raw material, also can be by adding the boracic raw material containing scandium raw material or carbon containing of carbon containing, as norbide.As long as the carbon adding is easy to participate in reaction under high temperature sintering condition, other materials in raw material can be taken away to reaction system with gas form, all can.
When containing scandium raw material, be Scium trioxide, when boracic raw material is norbide, by Sc
2o
3+ B
4c → ScB
2+ CO ↑+BO ↑+CO
2↑+B
2o
2↑ react, in products therefrom, except other materials of two scandium borides all leave with gas form, thereby can obtain two pure scandium borides.When being Scium trioxide containing scandium raw material, boracic raw material is norbide, when carbon raw material is carbon simple substance, by Sc
2o
3+ B
4c+C → ScB
2+ CO ↑ reacting, owing to only generating CO (carbon monoxide converter) gas, thereby gained two scandium boride purity are protected.
Carbon raw material is preferably the group that comprises the arbitrary or any number of compositions of graphite, carbon black or gac.These materials are pulverous carbon simple substance, can directly bring into play the effect of catalytic reduction.The add-on of carbon raw material is greater than zero.Scandium containing scandium raw material: the boron of boracic raw material: the carbon of carbon raw material is 1: 0.35～5: 0～3.5 mixing in molar ratio, and the carbon of carbon raw material is greater than in molar ratio zero and is less than 3.5 add-ons.In this ratio, add carbon raw material can guarantee that carbon raw material gives full play to the waste that raw material is avoided again in catalytic reduction effect, carrying out that can also accelerated reaction, improves the purity of two scandium borides.Preferably, raw material is 1: 2～4: 0～2.5 mixing containing scandium raw material, boracic raw material, carbon raw material by the mol ratio of Sc, B and C.In this ratio, mix obtained two scandium boride purities more than 99%.
In preparation process, sintering temperature is 1350～2000 ℃, by this temperature, can guarantee carrying out smoothly of reaction, if temperature is too low, reaction cannot occur, and can not generate two scandium boron.If excess Temperature, can cause the waste of the energy, increase the generation of the side reaction in reaction process, reduce the purity of gained material.Though by this temperature range react can guarantee reaction generation gained two scandium boride purity are lower.More Senior Two scandium boride purity should be higher to it has been generally acknowledged that sintering temperature, but reality be when sintering temperature during the closer to 1500 ℃ in products therefrom the purity of two scandium borides higher.Further preferably sintering temperature is 1500～1850 ℃, by these temperature sintering gained two scandium boride purity, is improved.Optimum sintering temperature is 1680～1750 ℃.The purity 99% of two scandium borides now.
Sintering time can carry out appropriateness test according to conventional experience and obtain a rational scope.This is because the length of sintering time can affect the degree of carrying out of reaction, and when temperature is elevated to preset range, reaction starts to occur, but just cooling soon after reaction starts, reaction can not fully be carried out, the residual products that mix with raw material in a large number of meeting, gained material separating-purifying difficulty.And can waste energy when sintering time is long.Thereby preferably, sintering time is 1～5 hour.By this time sintering, neither can waste energy and can guarantee that raw material fully reacts.Preferred sintering time is 1～3 hour, and now raw material reaction is the most abundant, gained two scandium boride purities 99%.
When being block, raw material can prepare two scandium borides equally.Owing to being sintered to solid state reaction, raw material granularity size all has impact to the purity of gained material and level of response.When raw material particle size is less than 270 microns, powder is more even after mixing, and contacts with each other fully after the little mixing of material particular diameter, and contact area is large, and be conducive to be swift in response, carry out fully, thus the purity of raising product.When the particle diameter of raw material thing is less than 270 microns, the purity 99% of gained two scandium borides.Because the particle diameter of raw material all has impact to the carrying out of reaction and the purity of final product.Preferably mixed material is carried out to compressing tablet processing, to strengthen in raw material the contact area between each component powders and to contact the degree of depth, deepen the carrying out of reaction, thereby improve the carrying out of reaction.Sintering again after compressing tablet is processed, the purity 99% of gained two scandium borides.Compressing tablet carries out according to a conventional method.Mixing raw material step can be mixed for hand operated mixing, mechanical stirring is mixed, the various conventional mixing meanss such as mixing or ball milling mixing of mediating, sieve.For promoting the mixing uniformity of raw material, preferably use ball milling to mix.Adopt ball milling to mix and can promote raw material mixing the particle diameter of raw material further to be reduced by the grinding of ball-milling medium again, and can also push each feed particles in mechanical milling process, it is adjacent to even each other and embeds, be conducive to the generation of subsequent reactions.In order to prevent the introducing of impurity element, the preferred corundum of liner of ball mill.
Sintering is to carry out in reaction crucible, and crucible material can be selected the high temperature materials such as graphite, tantalum, molybdenum, these materials not with reactant reaction.Sintering adds thermal recovery vacuum resistance furnace or carbon tube furnace carries out, and in sintering process, by 5～20 ℃/min, heats up.After oversintering, gained two scandium borides are easy to fragmentation, obtain powder after simple crushing.
Embodiment
In following examples, each material used and instrument are commercially available.
Used in following examples is that Scium trioxide, scandium fluoride, Scium trichloride, Scium trinitrate, acetic acid scandium and scandium carbonate or scandium are when arbitrary containing scandium raw material, need if desired first by the method in CN200910206271, to be undertaken after co-precipitation is treated to Scium trioxide coming into operation, raw materials used while taking raw material is that Scium trioxide, scandium fluoride, Scium trichloride, Scium trinitrate, acetic acid scandium and scandium carbonate or scandium are arbitrary again.
Embodiment 1
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
4the mol ratio of C: C is 1: 1: 2 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 99%.
Embodiment 2
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%), carbon dust (analytical pure) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
4the mol ratio of C: C is 1: 1.2: 1.5 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1700 ℃, be incubated 3 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 99%.
Embodiment 3
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%), activated carbon powder (analytical pure) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
4the mol ratio of C: C is 1: 2: 2.5 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1750 ℃, be incubated 4 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 99%.
Embodiment 4
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
4the mol ratio of C: C is 1: 1.5: 0.001 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 99%.
Embodiment 5
Take scandium fluoride (being greater than 99%), boron (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 340 microns, by containing scandium raw material: boracic raw material: the mol ratio of carbon raw material is 1: 0.65: 2 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1500 ℃, insulation hour, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 82%.
Embodiment 6
Take scandium fluoride (being greater than 99%), boron (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 500 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1: 5: 3.5 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 2000 ℃, be incubated 5 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 50%.
Embodiment 7
Take scandium fluoride (being greater than 99%), boron (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 70 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1: 2: 2.5 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1850 ℃, be incubated 3 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 70%.
Embodiment 8
Take Scium trinitrate (being greater than 99%), boric acid (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 300 microns, by containing scandium raw material: boracic raw material: the mol ratio of carbon raw material is 1: 0.74: 3.2 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1750 ℃, be incubated 1 hour, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 30%.
Embodiment 9
Take Scium trinitrate (being greater than 99%), boric acid (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1: 2: 0.001 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1680 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 50%.
Embodiment 10
Take Scium trinitrate (being greater than 99%), boric acid (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 400 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1: 3: 1.4 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1760 ℃, be incubated 4 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 65%.
Embodiment 11
Take acetic acid scandium (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 700 microns, by containing scandium raw material: boracic raw material: in carbon raw material, Sc, B and C mol ratio are 1:2.7:0.4 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1510 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 70%.
Embodiment 12
Take acetic acid scandium (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 220 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1:3.2:2 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1630 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 65%.
Embodiment 13
Take acetic acid scandium (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 210 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1:0.9:3.4 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1750 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 54%.
Embodiment 14
Take scandium carbonate (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 100 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1:1.2:2.3 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1490 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 52%.
Embodiment 15
Take scandium carbonate (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 110 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1:2:0.04 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1530 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 55%
Embodiment 16
Take scandium carbonate (being greater than 99%), norbide (being greater than 99%), Graphite Powder 99 (analytical pure) is raw material, the granularity of raw material is less than 270 microns, by containing scandium raw material: boracic raw material: in carbon raw material, the mol ratio of Sc, B and C is 1:3:0.3 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1720 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 60%.
Embodiment 17
Take scandium (being greater than 99%), boron (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by scandium: the mol ratio of boron is 1:1 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1780 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 60%.
Embodiment 18
Take scandium (being greater than 99%), boron (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by scandium: the mol ratio of boron is 1:2 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1720 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 90%.
Embodiment 19
Take scandium (being greater than 99%), boron (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by scandium: the mol ratio of boron is 1:2.2 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1730 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 95%.
Embodiment 20
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by containing Sc
2o
3: B
4the mol ratio of C is 1:0.7 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 65%.
Embodiment 21
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
4the mol ratio of C is 1:2.5 batching, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 75%.
Embodiment 22
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
4the mol ratio of C is 1:1 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 82.5%.
Embodiment 23
Take Scium trioxide (being greater than 99%), norbide (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
4the mol ratio of C is 1:1.25 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 90%.
Embodiment 24
Take Scium trioxide (being greater than 99%), boric acid (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: H
3bO
3mol ratio be 1:2 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 50%.
Embodiment 25
Take Scium trioxide (being greater than 99%), boron oxide (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: H
3bO
3mol ratio be 1:4 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 80%.
Embodiment 26
Take Scium trioxide (being greater than 99%), boron (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: H
3bO
3mol ratio be 1:5 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 85%.
Embodiment 27
Take scandium fluoride (being greater than 99%), norbide (being greater than 99%) is raw material, and 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 batching, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 50%.
Embodiment 28
Take scandium fluoride (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 65%.
Embodiment 29
Take scandium fluoride (being greater than 99%), norbide (being greater than 99%) is raw material, and 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 batching, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 80%.
Embodiment 30
Take Scium trichloride (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 60%.
Embodiment 31
Take Scium trichloride (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 80%.
Embodiment 32
Take Scium trichloride (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 72%.
Embodiment 33
Take Scium trinitrate (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 70%.
Embodiment 34
Take Scium trinitrate (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 80%.
Embodiment 35
Take Scium trinitrate (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 55%.
Embodiment 36
Take acetic acid scandium (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 60%.
Embodiment 37
Take acetic acid scandium (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 50%.
Embodiment 38
Take acetic acid scandium (being greater than 99%), norbide (being greater than 99%) is 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 56%.
Embodiment 39
Take Scium trioxide (being greater than 99%), boron oxide (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
2o
3mol ratio be 1:1.6 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 40%.
Embodiment 40
Take Scium trioxide (being greater than 99%), boron oxide (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
2o
3mol ratio be 1:2 batching, grind and fully mix rear compressing tablet, pack in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 70%.
Embodiment 41
Take Scium trioxide (being greater than 99%), boron oxide (being greater than 99%) is raw material, and 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 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 80%.
Embodiment 42
Take Scium trioxide (being greater than 99%), boron oxide (being greater than 99%), gac (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
2o
3: the mol ratio of C is 1:2:1 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 70%.
Embodiment 43
Take Scium trioxide (being greater than 99%), boron oxide (being greater than 99%), gac (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
2o
3: the mol ratio of C is 1:2.2:1 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 75%.
Embodiment 44
Take Scium trioxide (being greater than 99%), boron oxide (being greater than 99%), gac (being greater than 99%) is raw material, and the granularity of raw material is less than 270 microns, by Sc
2o
3: B
2o
3: the mol ratio of C is 1:2.2:1.5 batching, grinds and fully mixes rear compressing tablet, packs in reaction crucible.Then be placed in resistance furnace, under vacuum condition, with the temperature rise rate of 5～20 ℃/min, rise to 1600 ℃, be incubated 2 hours, cooling down then, the ScB obtaining
2through grinding to sieve, just make finished product ScB
2powder, purity is greater than 90%.
By embodiment 1～4 gained ScB
2powder is measured powder diffraction analysis collection of illustrative plates as shown in Figure 1, two scandium boride typical curve contrasts of two scandium boride sample curves and this curve below are known, and the peak (001) (100) (101) (002) (110) (102) (111) (200) (201) on two scandium boride sample curves all can be corresponding with the peak on two scandium boride typical curves.Illustrate that products therefrom is the ScB that purity is higher
2powder.
Embodiment 5～44 products therefroms are measured powder diffraction analysis collection of illustrative plates, find all two scandium borides can be detected in products therefrom, in product, two scandium boride content are minimum also can reach 30%, two scandium borides that purity is high that make that method energy simple and effective provided by the invention is described 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 a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (17)
1. a preparation method for two scandium borides, is characterized in that, comprises and will mix containing scandium raw material and boracic raw material, and sintering obtains described two scandium borides; Described is 1: 0.35～5 containing the scandium of scandium raw material and the boron mol ratio of described boracic raw material.
2. preparation method according to claim 1, is characterized in that, described containing scandium raw material scandium and the mol ratio of the boron of boracic raw material be 1: 2～4.
3. preparation method according to claim 1 and 2, is characterized in that, carbon raw material is mixed containing scandium raw material and boracic raw material with described.
4. preparation method according to claim 3, is characterized in that, 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: 0.35～5: 0～3.5.
5. preparation method according to claim 4, is characterized in that, 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.
6. according to the preparation method described in any one in claim 1～5, it is characterized in that, describedly containing scandium raw material, be selected from Scium trioxide, scandium fluoride, Scium trichloride, Scium trinitrate, acetic acid scandium and scandium carbonate or scandium is arbitrary or the group of any number of compositions.
7. preparation method according to claim 6, is characterized in that, described is Scium trioxide containing scandium raw material.
8. according to the preparation method described in any one in claim 1～5, it is characterized in that, described boracic raw material is selected from the group of arbitrary in boron, boron oxide, boric acid, norbide or any number of compositions.
9. preparation method according to claim 8, is characterized in that, described boracic raw material is norbide.
10. according to the preparation method described in any one in claim 3～5, it is characterized in that, described carbon raw material is selected from the group of the arbitrary or any number of compositions of graphite, carbon black or gac.
11. according to the preparation method described in any one in claim 1～10, it is characterized in that, described sintering temperature is 1500～2000 ℃.
12. preparation methods according to claim 11, is characterized in that, described sintering temperature is 1500～1850 ℃.
13. preparation methods according to claim 12, is characterized in that, described sintering temperature is 1680～1750 ℃.
14. according to the preparation method described in any one in claim 11～13, it is characterized in that, described sintering time is 1～5 hour.
15. preparation methods according to claim 14, is characterized in that, described sintering time is 1～3 hour.
16. according to the preparation method described in any one in claim 1～15, it is characterized in that, described raw material granularity is less than 270 microns.
17. preparation methods according to claim 16, is characterized in that, also comprise the step of compressing tablet after described mixing raw material step.
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