CN112062575A - A kind of10ZrB with uniformly controllable B abundance2Method for preparing powder - Google Patents

A kind of10ZrB with uniformly controllable B abundance2Method for preparing powder Download PDF

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CN112062575A
CN112062575A CN201911014522.6A CN201911014522A CN112062575A CN 112062575 A CN112062575 A CN 112062575A CN 201911014522 A CN201911014522 A CN 201911014522A CN 112062575 A CN112062575 A CN 112062575A
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powder
zrb
abundance
preparation
mixing
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王星明
杨磊
刘宇阳
白雪
彭程
桂涛
石志霞
孙静
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GRINM Resources and Environment Technology Co Ltd
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GRIMN Engineering Technology Research Institute Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
    • C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
    • C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures

Abstract

The invention discloses a10ZrB with uniformly controllable B abundance2A preparation method of powder belongs to the technical field of boride powder preparation. The method comprises the following steps: (1) preparation is different10ZrB abundant in B2Powder; (2) each different by acid washing10ZrB abundant in B2Purifying the powder; (3) by using intensive mixing of different10ZrB abundant in B2Powder preparation10Mixing is controlled by the uniformity of B abundance to obtain10ZrB with uniform B abundance distribution height2Powder; (4) using the differences obtained in step (3)10ZrB abundant in B2Powder, preparing and mixing to obtain the target10ZrB abundant in B2And (3) powder. The method has simple process, and can obtain10ZrB with stable and controllable B abundance, good uniformity and high purity2The purity of the powder is more than 99.9 percent,10the abundance value of B is controllable from 10 to 99 wt.%,10b abundance deviation was < 0.5 wt.%.

Description

A kind of10ZrB with uniformly controllable B abundance2Method for preparing powder
Technical Field
The invention relates to a10ZrB with uniformly controllable B abundance2A preparation method of powder belongs to the technical field of boride powder preparation.
Background
ZrB2The ceramic has the characteristics of high melting point, high hardness, good electric and heat conducting properties and the like, so that the ceramic is widely applied to the fields of high-temperature structural ceramic materials, composite materials, refractory materials, electrode materials, nuclear energy materials and the like. When ZrB2In (B) to10When B-enriched form exists, has excellent neutron absorption capacity, so that10B enriched ZrB2Fuel elements find application in nuclear reactors.
ZrB2There are various methods for preparing the powder, including a direct synthesis method, a self-propagating high-temperature synthesis method, a sol-gel method, a carbothermic method, and the like. However, due to the complexity of B-isotopology, prepared by the above method10B enriched ZrB2Powder, method for producing powder10The stability of the abundance of B is poor,10the B abundance distribution is not uniform. As shown in Table 1, 10 batches of ZrB prepared by carbothermic reduction2The powder is prepared by mixing the components of the powder,10the extreme difference of the B abundance value is 5.23, and the standard deviation is 1.84, which indicates that ZrB prepared from different batches2Of powders10Poor stability of B abundance and failure to satisfy nuclear reactor pairs10B enriched ZrB2The use requirements of the material. Thus solving the problems10B enriched ZrB2Powder body10B abundance stability and uniformity is preparation10B enriched ZrB2The powder needs to solve the problems.
TABLE 110 preparation by carbothermic processZrB2Powder body10B abundance value
Figure BDA0002243925690000011
Disclosure of Invention
The invention aims to solve the problem of the prior ZrB2The deficiency of the powder preparation technology provides10ZrB with uniformly controllable B abundance2A method for preparing powder.
In order to achieve the purpose, the invention adopts the following technical scheme:
a kind of10ZrB with uniformly controllable B abundance2The preparation method of the powder comprises the following steps:
(1) preparation is different10ZrB abundant in B2Powder;
(2) each different by acid washing10ZrB abundant in B2Purifying the powder;
(3) by using intensive mixing of different10ZrB abundant in B2Powder preparation10Mixing is controlled by the uniformity of B abundance to obtain10ZrB with uniform B abundance distribution height2Powder;
(4) using the differences obtained in step (3)10ZrB abundant in B2Powder, preparing and mixing to obtain the target10ZrB abundant in B2And (3) powder.
The preparation in the step (1) is different10ZrB abundant in B2The powder preparation method comprises a direct synthesis method, a self-propagating high-temperature synthesis method, a sol-gel method, a carbothermic method and the like.
ZrB prepared in the step (1)2Of powders10The B abundance value is 10-99 wt.%.
The step (2) is to perform acid pickling on ZrB2Purifying the powder, and pickling with a mixed solution of hydrochloric acid and nitric acid or hydrochloric acid and hydrogen peroxide; the concentration of hydrochloric acid is 1-3 mol/L, the concentration of nitric acid is 1-3 mol/L, and the concentration of hydrogen peroxide is 1-10 mol/L; the volume ratio of the hydrochloric acid to the nitric acid is (3-5) to 1,the ratio of the hydrochloric acid to the hydrogen peroxide is (1-10) to 1.
ZrB in the step (3)2The mixing mode of the powder is high-speed intensive mixing or three-dimensional motion mixing; using a high-speed intensive mixing mode to treat different diseases10ZrB abundant in B2Mixing the powder, wherein the rotating speed of a mixer is 300-1500 r/min, and the mixing time is 10-120 min; using a three-dimensional motion mixing mode to correct for differences10ZrB abundant in B2And mixing the powder, wherein the rotating speed of a main shaft of the mixer is 5-30r/min, and the mixing time is 30-240 min.
Preparing and mixing in the step (4) to obtain the target10ZrB abundant in B2The powder is mixed by the high-speed intensive mixing or three-dimensional motion mixing method.
The invention has the advantages that:
the ZrB is improved through the pickling purification process2The purity of the powder; and adopts a method of intensive mixing to realize10B enriched ZrB2Of powders10B abundance stability control to obtain10ZrB with stable and controllable B abundance, good uniformity and high purity2And (3) powder. The concrete expression is as follows:
(1) the invention adopts acid pickling to ZrB2The powder is purified, so that the content of impurity elements in the powder is effectively reduced, and the purity of the powder is more than 99.9 percent;
(2) the invention adopts a high-speed strong mixing or three-dimensional motion mixing method to realize ZrB2Of powders10The abundance of the B is stable and controllable, and the uniformity is high,10the abundance value of B is controllable from 10 to 99 wt.%,10b abundance deviation was < 0.5 wt.%.
Drawings
FIG. 1 is a drawing of10ZrB with uniformly controllable B abundance2And (3) powder preparation process.
Detailed Description
The invention is further illustrated with reference to the following figures and examples. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
As shown in fig. 1, the invention provides10ZrB with uniformly controllable B abundance2The preparation process of the powder comprises the following steps: preparation is different10ZrB abundant in B2Powder; pickling of ZrB2Purifying the powder; ZrB realization by adopting intensive mixing method2In the powder10Mixing is controlled by the high uniformity of B abundance; weighing the ZrB by material proportioning calculation2Powder of, is subjected to10B abundance is prepared and mixed to obtain a target10ZrB abundant in B2And (3) powder.
Example 1:10ZrB with a B abundance of 10 wt%2Preparation of powder
Prepared by carbothermic method10ZrB abundant in B220kg of powder ZrB2Theory of powder10B abundance value is 10 wt.%, 10-point sampling measurement is carried out on the powder10B abundance, the results are shown in Table 3,10b abundance deviation was max 1.36 wt.%; the ZrB is treated by using a mixed solution of 1mol/L hydrochloric acid and 1mol/L nitric acid2Pickling the powder, wherein the volume ratio of hydrochloric acid to nitric acid is 3: 1; mixing the powder after the acid washing by adopting a high-speed mixer, wherein the rotating speed of the mixer is 1500r/min, and the mixing time is 10min to obtain10ZrB with uniform B abundance2The purity of the powder is more than 99.9 percent (shown in a table 2),10b abundance deviated by < 0.4 wt.% (as shown in table 3).
Table 2 example 1 related ZrB2Analysis result of powder purity
Impurity element Content/ppm Impurity element Content/ppm Impurity element Content/ppm
Mg 3 A1 45 Si 46
Ca 70 V ＜10 Cr 10
Mn ＜5 Fe 76 Ni ＜5
Co ＜5 Cu ＜3 Zn ＜5
As ＜1 Mo 20 Cd ＜3
Sn ＜1 Sb ＜10 Pb ＜5
Table 3 example 1 related ZrB2Of powders10Measured B abundance
Figure BDA0002243925690000031
Example 2:10ZrB with a B abundance of 30 wt%2Preparation of powder
Prepared by a sol-gel method10ZrB with a B abundance of 18.5 wt%25kg of powder prepared by carbothermic method10ZrB with a B abundance of 55 wt%220kg of powder, 10-point sampling and measuring of the powder10B abundance, results are shown in table 5; the two ZrB are treated by using a mixed solution of 3mol/L hydrochloric acid and 1mol/L nitric acid2Pickling the powder, wherein the volume ratio of hydrochloric acid to nitric acid is 1: 1; mixing the acid-washed powder by using a three-dimensional motion mixer respectively, wherein the rotating speed of a main shaft of the mixer is 25r/min, and the time is 30min to obtain 2 types of the acid-washed powder10ZrB with uniform B abundance distribution height2Powder, method for producing powder10B abundance deviation values were all < 0.5 wt.% (as shown in table 5); get10ZrB with a B abundance of 55 wt%2The powder is 6.3kg of the powder,10ZrB with a B abundance of 18.5 wt%2Mixing 13.7kg of powder by a high-speed mixer at the rotating speed of 1000r/min for 60min to obtain the powder10ZrB with a B abundance of 30 wt%220kg of powder, the purity of the powder is more than 99.9% (as shown in table 4,10b abundance deviated by < 0.3 wt.% (as shown in table 5).
Table 4 example 2 related ZrB2Analysis result of powder purity
Impurity element Content/ppm Impurity element Content/ppm Impurity element Content/ppm
Mg 6 A1 50 Si 50
Ca 75 V ＜10 Cr ＜5
Mn ＜5 Fe 66 Ni ＜5
Co ＜5 Cu ＜5 Zn ＜5
As ＜1 Mo ＜10 Cd ＜3
Sn ＜1 Sb ＜10 Pb ＜5
Table 5 example 2 related ZrB2Of powders10Measured B abundance
Figure BDA0002243925690000041
Example 3:10ZrB with a B abundance of 50 wt%2Preparation of powder
Respectively prepared by adopting a carbothermic method10ZrB with B abundance of 95 wt.%, 20 wt.% and 60 wt.%220kg of powder respectively; carrying out acid washing treatment on the prepared powder by using a mixed solution of 3mol/L hydrochloric acid and 1mol/L hydrogen peroxide, wherein the volume ratio of the hydrochloric acid to the hydrogen peroxide is 5: 1; mixing the acid-washed powder by a three-dimensional motion mixer at a main shaft rotating speed of 20r/minThe time is 60min, 3 kinds are obtained10ZrB with uniform B abundance distribution height2Powder, method for producing powder10B abundance deviation values were all < 0.5 wt.%; get10ZrB with a B abundance of 95 wt%2The weight of the powder is 5.714kg,10ZrB with a B abundance of 20 wt%210kg of powder is prepared by mixing the components of 10kg,10ZrB with a B abundance of 60 wt%24.286kg of powder is mixed by a high-speed mixer, the rotating speed of the mixer is 1300r/min, and the mixing time is 60min, so as to obtain the powder10ZrB with a B abundance of 50 wt%220kg of powder, the purity of the powder is more than 99.9 percent,10b abundance deviation was < 0.3 wt.%.
Example 4:10ZrB with a B abundance of 70 wt%2Preparation of powder
Prepared by carbothermic method10ZrB with a B abundance of 55 wt%210kg of powder prepared by carbothermic method10ZrB with a B abundance of 95 wt%210kg of powder; carrying out acid washing treatment by using a mixed solution of 1mol/L hydrochloric acid and 1mol/L hydrogen peroxide, wherein the volume ratio of the hydrochloric acid to the hydrogen peroxide is 3: 1; mixing the acid-washed powder with high-speed mixer at rotation speed of 800r/min for 30min to obtain 2 kinds of powder10ZrB with uniform B abundance distribution height2Powder, method for producing powder10B abundance deviation values were all < 0.5 wt.%; get10ZrB with a B abundance of 55 wt%2The powder is 6.25kg of the powder,10ZrB with a B abundance of 95 wt%23.75kg of powder is mixed by a high-speed mixer, the rotating speed of the mixer is 1200r/min, and the mixing time is 40min, so as to obtain the powder10ZrB with a B abundance of 70 wt%210kg of powder, the purity of the powder is more than 99.9 percent,10b abundance deviation was < 0.5 wt.%.
Example 5:10ZrB with a B abundance of 90 wt%2Preparation of powder
Prepared by adopting self-propagating high-temperature synthesis method10ZrB with a B abundance of 18.5 wt%25kg of powder prepared by carbothermic method10ZrB with a B abundance of 95 wt%220kg of powder; the two ZrB bodies are treated by a mixed solution of 3mol/L hydrochloric acid and 1mol/L nitric acid2The powder is subjected to an acid washing treatment in whichThe volume ratio of the hydrochloric acid to the nitric acid is 1: 1; mixing the acid-washed powder by using a three-dimensional motion mixer respectively, wherein the rotating speed of a main shaft of the mixer is 25r/min, and the time is 30min to obtain 2 types of the acid-washed powder10ZrB with uniform B abundance distribution height2Powder, method for producing powder10B abundance deviation values were all < 0.5 wt.%; get10ZrB with a B abundance of 95 wt%2The powder is 18.7kg of the powder,10ZrB with a B abundance of 18.5 wt%21.3kg of powder is mixed by a high-speed mixer, the rotating speed of the mixer is 1000r/min, and the mixing time is 60min, so as to obtain the powder10ZrB with a B abundance of 90 wt%220kg of powder, the purity of the powder is more than 99.9 percent,10b abundance deviation was < 0.3 wt.%.

Claims (7)

1. A kind of10ZrB with uniformly controllable B abundance2The preparation method of the powder is characterized by comprising the following steps:
(1) preparation is different10ZrB abundant in B2Powder;
(2) each different by acid washing10ZrB abundant in B2Purifying the powder;
(3) by using intensive mixing of different10ZrB abundant in B2Powder preparation10Mixing is controlled by the uniformity of B abundance to obtain10ZrB with uniform B abundance distribution height2Powder;
(4) using the differences obtained in step (3)10ZrB abundant in B2Powder, preparing and mixing to obtain the target10ZrB abundant in B2And (3) powder.
2. The method of claim 110ZrB with uniformly controllable B abundance2The preparation method of the powder is characterized in that the preparation in the step (1) is different10ZrB abundant in B2The powder is prepared by direct synthesis, self-propagating high-temperature synthesis, sol-gel method or carbothermic method.
3. The method of claim 110ZrB with uniformly controllable B abundance2The preparation method of the powder is characterized in that ZrB prepared in the step (1)2Of powders10The B abundance value is 10-99 wt.%.
4. The method of claim 110ZrB with uniformly controllable B abundance2The preparation method of the powder is characterized in that ZrB is subjected to acid washing in the step (2)2Purifying the powder, and pickling with a mixed solution of hydrochloric acid and nitric acid or hydrochloric acid and hydrogen peroxide; the concentration of hydrochloric acid is 1-3 mol/L, the concentration of nitric acid is 1-3 mol/L, and the concentration of hydrogen peroxide is 1-10 mol/L; the volume ratio of the hydrochloric acid to the nitric acid is (3-5) to 1, and the ratio of the hydrochloric acid to the hydrogen peroxide is (1-10) to 1.
5. The method of claim 110ZrB with uniformly controllable B abundance2The preparation method of the powder is characterized in that ZrB in the step (3) or the step (4)2The mixing mode of the powder is high-speed intensive mixing or three-dimensional motion mixing.
6. The method of claim 510ZrB with uniformly controllable B abundance2The preparation method of the powder is characterized in that when a high-speed intensive mixing mode is utilized, the rotating speed of a mixer is 300-1500 r/min, and the mixing time is 10-120 min; when a three-dimensional motion mixing mode is used, the rotating speed of a main shaft of the mixer is 5-30r/min, and the mixing time is 30-240 min.
7. The method of claim 110ZrB with uniformly controllable B abundance2A method for producing a powder, characterized by10B enriched ZrB2The purity of the powder is more than 99.9 percent.
CN201911014522.6A 2019-10-23 2019-10-23 A kind of10ZrB with uniformly controllable B abundance2Method for preparing powder Pending CN112062575A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114956832A (en) * 2022-04-02 2022-08-30 有研资源环境技术研究院(北京)有限公司 Ultrahigh-temperature ceramic densification method and ultrahigh-temperature ceramic

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
杨磊: "碳热还原反应制备ZrB2粉体工艺研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 *
桂涛: "10B富集的二硼化锆靶材制备", 《中国优秀博硕士学位论文全文数据库(博士)工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114956832A (en) * 2022-04-02 2022-08-30 有研资源环境技术研究院(北京)有限公司 Ultrahigh-temperature ceramic densification method and ultrahigh-temperature ceramic
CN114956832B (en) * 2022-04-02 2023-10-03 有研科技集团有限公司 Densification method of ultrahigh-temperature ceramic and ultrahigh-temperature ceramic

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