CN102259882B - Preparation method of high-purity YB4 powder body - Google Patents

Preparation method of high-purity YB4 powder body Download PDF

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Publication number
CN102259882B
CN102259882B CN 201110167435 CN201110167435A CN102259882B CN 102259882 B CN102259882 B CN 102259882B CN 201110167435 CN201110167435 CN 201110167435 CN 201110167435 A CN201110167435 A CN 201110167435A CN 102259882 B CN102259882 B CN 102259882B
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powder
raw material
purity
material powder
room temperature
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CN102259882A (en
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李俊国
何勇
袁辉平
郭启龙
张联盟
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a preparation method of YB4 powder body, which comprises the following steps of: 1) taking Y2O3 and B4C raw material powder and uniformly mixing; 2) pressing the uniformly mixed raw material powder into block bodies; then, putting the block bodies into a die; under a vacuum condition, raising the temperature to 1700 DEG C to 2000 DEG C; preserving the temperature for 15 to 120 minutes; then, cooling with a stove to room temperature; 3) taking out the obtained block bodies; grinding; putting the block bodies into hydrochloric acid; heating; stirring; filtering to be dry; washing with deionized water to be natural; and 4) drying the obtained powder body. According to the invention, commercially available Y2O3 and B4C powder is used as raw material, is easy to obtain and has low price; in the reaction process, element C and element O are combined for generating CO gas for volatilization; element Y and element B are combined for generating YB4; the introduction of other foreign matter is effectively avoided; high-purity YB4 powder body is obtained; the prepared YB4 has single phase; the size of crystal grain is from 3 to 10 mu m; and the product purity is higher than 99.5%.

Description

A kind of high-purity YB 4The preparation method of powder
Technical field
The present invention relates to YB 4The preparation method of powder belongs to material synthesis method, the YB that makes 4Powder can be applicable to the fields such as stupalith and electronic material.
Background technology
In recent years, boride has been carried out a large amount of research both at home and abroad.Because boride has good electroconductibility usually, very high hardness and fusing point can be used as electronic material and stupalith.
Prepare at present YB 4Method mainly contain four kinds: first method is to adopt pure metal Y and simple substance B, and at high temperature direct reaction obtains, and the advantage of this method is the YB that is synthesized 4Purity is very high, and can not introduce other impurity in the reaction process, and shortcoming is the very expensive and difficult acquisition of cost of material that this method is used, thereby can't realize scale operation; Second method is the hot method of boron, namely adopts Y 2O 3Powder and simple substance B are raw material, at high temperature synthetic YB 4, the YB that this method is synthetic 4Purity is higher, but makes raw material with B simple substance, and is expensive; The third method is the ratio by control Y, B, Al, the YB of preparation large-size 4Crystal, but not only the prices of raw and semifnished materials are expensive for this method, and also technique is comparatively complicated, is difficult to realize practical application; The 4th kind of method is the halogenide YCl with yttrium 37H 2O, simple substance B and Al are raw material, and be at high temperature directly synthetic, and comparatively expensive but the shortcoming of this method is cost of material, reaction process is comparatively complicated.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of low-cost preparation high-purity YB 4The preparation method of powder, employed cost of material is cheap, is easy to obtain, and is conducive to realize large-scale industrial production.
The present invention solves its technical problem and adopts following technical scheme: high-purity YB 4The preparation method of powder includes following steps:
1) gets Y 2O 3And B 4The C raw material powder, and mix, the proportioning of described raw material powder is mol ratio Y 2O 3: B 4C=1: 2.0～2.3;
2) raw material powder with mixing is pressed into block under 0～5MPa, and the mould of then packing into is 10 -2Under the vacuum condition of～1500Pa, be warming up to 1700～2000 ℃ and be incubated 15～120min, then cool to room temperature with the furnace;
3) taking-up of gained block is ground, then be placed in the hydrochloric acid, then heated and stirred is filtered dry it, extremely neutral with deionized water rinsing;
4) with the oven dry of gained powder, namely get high-purity YB 4Powder.
Press such scheme, the described concentration of hydrochloric acid of step 3) is 2mol/L～6mol/L, and pickling temperature is 60 ℃, and the time is 10～120min.
The present invention utilizes commercially available Y 2O 3And B 4The C powder is raw material, with existing YB 4Synthetic method is compared, and the present invention has that employed raw material be very easy to obtain and cheap remarkable advantage, and in the reaction process C element can and the O element in conjunction with generating the CO gaseous volatilization, Y element and B element are in conjunction with generation YB 4, thereby can effectively avoid the introducing of other impurity, obtain highly purified YB 4Powder utilizes the prepared YB of the present invention 4Phase is single, grain-size is 3～10 μ m, learns that through the oxygen nitrogen analysis wherein oxygen level all is lower than 0.5%, and product purity is higher than 99.5%.
Description of drawings
Fig. 1 is embodiment 2 described raw material powder and synthetic YB 4The XRD figure of (PDF 79-1992) powder;
Fig. 2 is embodiment 2 described synthetic YB 4The SEM figure of powder, wherein (a) is synthetic powder low power SEM figure, (b) is the clear SEM figure of synthetic powder high power.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Embodiment 1:
(1) with Y 2O 3And B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=take by weighing 4.47g at 1: 2.0, and in agate mortar mix grinding 3h;
(2) with the raw material powder of mixing at the right cylinder that is pressed into Φ 10 * 10mm on the powder compressing machine under with the pressure about 3MPa, and with in its graphite jig of packing into, utilize discharge plasma sintering system (SPS), (vacuum tightness of using among the embodiment is initial depression under the 20Pa vacuum condition, and the reaction process intermediate pump turns round always and vacuumizes), rise to 1700 ℃ from room temperature, and insulation 30min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 2mol/L, be heated to 60 ℃, stir 120min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.
Embodiment 2:
(1) with Y 2O 3And B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=take by weighing 4.54g at 1: 2.1, with mix grinding 3h in its agate mortar of packing into;
(2) with the raw material powder of mixing at the right cylinder that is pressed into Φ 10 * 10mm on the powder compressing machine under with the pressure about 3MPa, and with in its graphite jig of packing into, utilize discharge plasma sintering system (SPS), under the 20Pa vacuum condition, rise to 1700 ℃ from room temperature, and insulation 30min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 2mol/L, be heated to 60 ℃, stir 120min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.
Embodiment 3:
(1) with Y 2O 3Powder and B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=1: 2.3 4.69g that weighs adds mix grinding 3h in the agate mortar with it;
(2) raw material powder of mixing is directly packed in the graphite jig, utilize discharge plasma sintering system (SPS), under the 20Pa vacuum condition, rise to 1700 ℃ from room temperature, and insulation 30min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 2mol/L, be heated to 60 ℃, stir 10min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.
Embodiment 4:
(1) with Y 2O 3Powder and B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=1: 2.1 4.54g that weighs is with mix grinding 3h in its agate mortar of packing into;
(2) with the raw material powder of mixing at the right cylinder that is pressed into Φ 10 * 10mm on the powder compressing machine under with the pressure about 3MPa, and with in its graphite jig of packing into, utilize discharge plasma sintering system (SPS), under the 20Pa vacuum condition, rise to 1800 ℃ from room temperature, and insulation 25min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 2mol/L, be heated to 60 ℃, stir 120min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.
Embodiment 5:
(1) with Y 2O 3Powder and B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=1: 2.1 4.54g that weighs is with mix grinding 3h in its agate mortar of packing into;
(2) with the raw material powder of mixing at the right cylinder that is pressed into Φ 10 * 10mm on the powder compressing machine under with the pressure about 3MPa, and with in its graphite jig of packing into, utilize discharge plasma sintering system (SPS), under the 20Pa vacuum condition, rise to 1900 ℃ from room temperature, and insulation 20min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 2mol/L, be heated to 60 ℃, stir 120min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.
Embodiment 6:
(1) with Y 2O 3Powder and B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=1: 2.1 4.54g that weighs is with mix grinding 3h in its agate mortar of packing into;
(2) with the raw material powder of mixing at the right cylinder that is pressed into Φ 10 * 10mm on the powder compressing machine under with the pressure about 3MPa, and with in its graphite jig of packing into, utilize discharge plasma sintering system (SPS), under the 1000Pa vacuum condition, rise to 1900 ℃ from room temperature, and insulation 30min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 2mol/L, be heated to 60 ℃, stir 120min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.
Embodiment 7:
(1) with Y 2O 3Powder and B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=1: 2.1 4.54g that weighs is with mix grinding 3h in its agate mortar of packing into;
(2) raw material powder of mixing is pressed into the right cylinder of Φ 10 * 10mm under with the pressure about 3MPa on the powder compressing machine, and with in its graphite jig of packing into, is utilizing vacuum sintering funace, 10 -1Under the Pa vacuum condition, rise to 1900 ℃ from room temperature, and insulation 60min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 2mol/L, be heated to 60 ℃, stir 120min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.
Embodiment 8:
(1) with Y 2O 3Powder and B 4The C powder is at 200 ℃ of lower dry 5h, then with Y 2O 3And B 4Two kinds of raw material powder of C are Y in molar ratio 2O 3: B 4C=1: 2.1 4.54g that weighs is with mix grinding 3h in its agate mortar of packing into;
(2) with the raw material powder of mixing at the right cylinder that is pressed into Φ 10 * 10mm on the powder compressing machine under with the pressure about 3MPa, and with in its graphite jig of packing into, utilize discharge plasma sintering system (SPS), under the 20Pa vacuum condition, rise to 1700 ℃ from room temperature, and insulation 30min, then cool to room temperature with the furnace;
(3) the gained block is taken out, in agate mortar, grind, then be placed in the dilute hydrochloric acid of 6mol/L, be heated to 60 ℃, stir 30min with stirrer, then be filtered dry, repeatedly wash to neutrality with deionized water;
(4) powder that makes is placed loft drier, at 100 ℃ of oven dry 2h, namely obtain high-purity YB 4Powder.

Claims (2)

1. high-purity YB 4The preparation method of powder is characterized in that including following steps:
1) gets Y 2O 3And B 4The C raw material powder, and mix, the proportioning of described raw material powder is mol ratio Y 2O 3: B 4C=1: 2.0～2.3;
2) raw material powder with mixing is pressed into block under 3～5MPa, and the mould of then packing into is 10 -2Under the vacuum condition of～1500Pa, be warming up to 1700～2000 ℃ and be incubated 15～120min, then cool to room temperature with the furnace;
3) taking-up of gained block is ground, then be placed in the hydrochloric acid, then heated and stirred is filtered dry it, extremely neutral with deionized water rinsing;
4) with the oven dry of gained powder, namely get high-purity YB 4Powder.
2. by high-purity YB claimed in claim 1 4The preparation method of powder is characterized in that the described concentration of hydrochloric acid of step 3) is 2mol/L～6mol/L, and pickling temperature is 60 ℃, and the time is 10～120min.
CN 201110167435 2011-06-21 2011-06-21 Preparation method of high-purity YB4 powder body Expired - Fee Related CN102259882B (en)

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CN103896297A (en) * 2014-04-09 2014-07-02 湖南稀土金属材料研究院 Preparation method of yttrium tetraboride
CN106866152B (en) * 2017-03-10 2019-09-03 北京工业大学 A kind of YB4The preparation method of block

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330942A (en) * 1993-01-22 1994-07-19 Martin Marietta Energy Systems, Inc. Composite of refractory material
CN101948117A (en) * 2010-10-11 2011-01-19 山东大学 Method for preparing nano superfine rare-earth hexaboride powder
CN102050457A (en) * 2009-10-29 2011-05-11 苏玉长 Synthesis method of nano rare-earth tetraboride and applications thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330942A (en) * 1993-01-22 1994-07-19 Martin Marietta Energy Systems, Inc. Composite of refractory material
CN102050457A (en) * 2009-10-29 2011-05-11 苏玉长 Synthesis method of nano rare-earth tetraboride and applications thereof
CN101948117A (en) * 2010-10-11 2011-01-19 山东大学 Method for preparing nano superfine rare-earth hexaboride powder

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