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CN104437155A - Dispersing method for ZrB2 nanopowder - Google Patents

Dispersing method for ZrB2 nanopowder Download PDF

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Publication number
CN104437155A
CN104437155A CN201410631888.9A CN201410631888A CN104437155A CN 104437155 A CN104437155 A CN 104437155A CN 201410631888 A CN201410631888 A CN 201410631888A CN 104437155 A CN104437155 A CN 104437155A
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China
Prior art keywords
zrb2
powder
zrb2 powder
solvent
nanometer
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CN201410631888.9A
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Chinese (zh)
Inventor
程业红
张幸红
韩文波
胡平
洪长青
安家东
王鹏
赵广东
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Harbin Institute of Technology
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Harbin Institute of Technology
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Priority to CN201410631888.9A priority Critical patent/CN104437155A/en
Publication of CN104437155A publication Critical patent/CN104437155A/en
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Abstract

The invention relates to a dispersing method for ZrB2 nanopowder and aims at solving the problem that the ZrB2 nanopowder is easily agglomerated in water. The dispersing method comprises the steps of firstly, titrating deionized water by using acid or alkaline to obtain a solvent with the pH value of 3 or 11; and secondly, weighing ZrB2 powder and a dispersing agent, sequentially adding the ZrB2 powder and the dispersing agent into the solvent, and carrying out ultrasonic treatment for 14-16 minutes to obtain uniformly-dispersed slurry, namely finishing the dispersion of the ZrB2 nanopowder. By using the dispersing method disclosed by the invention, the dispersing effect is good, the ZrB2 nanopowder can be uniformly dispersed, and the slurry cannot be remarkably settled within 24 hours. The agglomeration size of the ZrB2 nanopowder is relatively small, the agglomeration size of the ZrB2 powder is smaller than 300nm, and the Zeta potential is about 40mv. The dispersing method is applied to the field of nanomaterials.

Description

The method of dispersing nanometer ZrB2 powder
Technical field
The present invention relates to the process for dispersing of nanometer ZrB2 powder.
Background technology
Nano material, because its crystallite dimension is in nanometer scale, makes its some performance have the peculiar advantage being different from traditional material, as high mechanical property, high rigidity, superplasticity and the property in acousto-optic-electric is pyromagnetic.ZrB2, due to its high high temperature resistant, anti-oxidant, anti-yaw damper performance, is considered to hypersonic flight, the optimal candidate material of the extreme chemical environment that Reentry is relevant with rocket propulsion and thermal environment.Noted by gel and prepare ceramic material, have can prepare complex structural member, base substrate is convenient to mach advantage.Gel injection-moulding prepares nanometer ZrB2 becomes a kind of new preparation method.When utilizing gel injection-moulding to prepare nanometer ZrB2-SiC material, because the surface area ratio of nanometer ZrB2 powder is comparatively large, be easy in a solvent reunite.
Summary of the invention
The present invention is the problem that will solve the easily reunion in water of nanometer ZrB2 powder, provides a kind of method of dispersing nanometer ZrB2 powder.
The method of dispersing nanometer ZrB2 powder of the present invention, carry out according to the following steps:
One, obtain by acidometric titration deionized water the solvent that pH is 3;
Two, take ZrB2 powder and dispersant, successively join in solvent by ZrB2 powder and dispersant, ultrasonic 14 ~ 16min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
The method of the present invention another kind of dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by alkalimetric titration deionized water the solvent that pH is 11;
Two, take ZrB2 powder and dispersant, successively join in solvent by ZrB2 powder and dispersant, ultrasonic 14 ~ 16min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
The present invention has the following advantages:
1, the solvent that the present invention uses is deionized water, and inexpensive clean is pollution-free.
2, the dispersion effect of the inventive method good, be uniformly dispersed, obvious sediment can be there is not by 24h in slurry.
3, the agglomerate size of nanometer ZrB2 powder is less, and the agglomerate size of ZrB2 powder is less than 300nm, and Zeta potential is about 40mv.
When ZrB2 powder after the inventive method dispersion prepares nanometer ZrB2-SiC material for gel injection-moulding, not easily reunite.
Accompanying drawing explanation
Fig. 1 is the slurry original state figure being dispersed with ZrB2 that embodiment 1 ~ 3 obtains; Fig. 2 is that the slurry being dispersed with ZrB2 that embodiment 1 ~ 3 obtains leaves standstill the effect after 24 hours; Fig. 3 is the slurry original state figure being dispersed with ZrB2 that embodiment 4 ~ 6 obtains; Fig. 4 is that the slurry being dispersed with ZrB2 that embodiment 4 ~ 6 obtains leaves standstill the effect after 24 hours.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: the method for present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by acidometric titration deionized water the solvent that pH is 3;
Two, take ZrB2 powder and dispersant, successively join in solvent by ZrB2 powder and dispersant, ultrasonic 14 ~ 16min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: in step one, acid is lactic acid.Other is identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two unlike: in step 2, the particle diameter of ZrB2 powder is 50 ~ 100nm, and purity is greater than 99%.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: in step 2, dispersant is polymine (PEI).Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike: in step 2, the quality of ZrB2 powder is 2% of solvent quality, and the quality of dispersant is 2% ~ 6% of ZrB2 powder quality.Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: the method for present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by alkalimetric titration deionized water the solvent that pH is 11;
Two, take ZrB2 powder and dispersant, successively join in solvent by ZrB2 powder and dispersant, ultrasonic 14 ~ 16min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
Detailed description of the invention seven: present embodiment and detailed description of the invention six unlike: in step one, alkali is ammoniacal liquor.Other is identical with detailed description of the invention six.
Detailed description of the invention eight: present embodiment and detailed description of the invention six or seven unlike: in step 2, the average grain diameter of ZrB2 powder is 100nm, and purity is greater than 99%.Other is identical with detailed description of the invention six or seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention six to eight unlike: in step 2, dispersant is ammonium polyacrylate (PAA-NH4).Other is identical with one of detailed description of the invention six to eight.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention six to nine unlike: in step 2, the quality of ZrB2 powder is 2% of solvent quality, and the quality of dispersant is 2% ~ 6% of ZrB2 powder quality.Other is identical with one of detailed description of the invention six to nine.
Embodiment 1:
The method of the present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by lactic acid titration deionized water the solvent that pH is 3;
Two, take 0.2gZrB2 powder and 0.004g polymine, successively join in 10mL solvent by ZrB2 powder and polymine, ultrasonic 15min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
In step 2, the average grain diameter of ZrB2 powder is 100nm, and purity is greater than 99%.
In step 2, polyethylene of dispersing agent imines is for analyzing pure grade.
Ultrasonic power described in step 2 is 100w, and frequency is 180khz.
Embodiment 2:
The method of the present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by lactic acid titration deionized water the solvent that pH is 3;
Two, take 0.2gZrB2 powder and 0.008g polymine, successively join in 10mL solvent by ZrB2 powder and polymine, ultrasonic 15min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
In step 2, the average grain diameter of ZrB2 powder is 100nm, and purity is greater than 99%.
In step 2, polyethylene of dispersing agent imines is for analyzing pure grade.
Ultrasonic power described in step 2 is 100w, and frequency is 180khz.
Embodiment 3:
The method of the present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by lactic acid titration deionized water the solvent that pH is 3;
Two, take 0.2gZrB2 powder and 0.012g polymine, successively join in 10mL solvent by ZrB2 powder and polymine, ultrasonic 15min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
In step 2, the average grain diameter of ZrB2 powder is 100nm, and purity is greater than 99%.
In step 2, polyethylene of dispersing agent imines is for analyzing pure grade.
Ultrasonic power described in step 2 is 100w, and frequency is 180khz.
Embodiment 4:
The method of the present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by ammonia water titration deionized water the solvent that pH is 11;
Two, take 0.2gZrB2 powder and 0.004g ammonium polyacrylate, successively join in 10mL solvent by ZrB2 powder and polymine, ultrasonic 15min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
In step 2, the average grain diameter of ZrB2 powder is 100nm, and purity is greater than 99%.
In step 2, dispersants ammonium polyacrylate is for analyzing pure grade.
Ultrasonic power described in step 2 is 100w, and frequency is 180khz.
Embodiment 5:
The method of the present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by ammonia water titration deionized water the solvent that pH is 11;
Two, take 0.2gZrB2 powder and 0.008g ammonium polyacrylate, successively join in 10mL solvent by ZrB2 powder and polymine, ultrasonic 15min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
In step 2, the average grain diameter of ZrB2 powder is 100nm, and purity is greater than 99%.
In step 2, dispersants ammonium polyacrylate is for analyzing pure grade.
Ultrasonic power described in step 2 is 100w, and frequency is 180khz.
Embodiment 6:
The method of the present embodiment dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by ammonia water titration deionized water the solvent that pH is 11;
Two, take 0.2gZrB2 powder and 0.012g ammonium polyacrylate, successively join in 10mL solvent by ZrB2 powder and polymine, ultrasonic 15min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
In step 2, the average grain diameter of ZrB2 powder is 100nm, and purity is greater than 99%.
In step 2, dispersants ammonium polyacrylate is for analyzing pure grade.
Ultrasonic power described in step 2 is 100w, and frequency is 180khz.
What embodiment 1 ~ 3 obtained is dispersed with the slurry original state figure of ZrB2 as shown in Figure 1, in Fig. 1, a is the slurry not adding dispersant, b is the slurry being dispersed with ZrB2 that embodiment 1 obtains, c is the slurry being dispersed with ZrB2 that embodiment 2 obtains, and d is the slurry being dispersed with ZrB2 that embodiment 3 obtains.The slurry of what embodiment 1 ~ 3 obtained be dispersed with ZrB2 leaves standstill the effect after 24 hours as shown in Figure 2, in Fig. 2, a is the slurry not adding dispersant, b is the slurry being dispersed with ZrB2 that embodiment 1 obtains, c is the slurry being dispersed with ZrB2 that embodiment 2 obtains, and d is the slurry being dispersed with ZrB2 that embodiment 3 obtains.
What embodiment 4 ~ 6 obtained is dispersed with the slurry original state figure of ZrB2 as shown in Figure 3, in Fig. 3, a is the slurry not adding dispersant, b is the slurry being dispersed with ZrB2 that embodiment 1 obtains, c is the slurry being dispersed with ZrB2 that embodiment 2 obtains, and d is the slurry being dispersed with ZrB2 that embodiment 3 obtains.The slurry of what embodiment 4 ~ 6 obtained be dispersed with ZrB2 leaves standstill the effect after 24 hours as shown in Figure 4, in Fig. 4, a is the slurry not adding dispersant, b is the slurry being dispersed with ZrB2 that embodiment 1 obtains, c is the slurry being dispersed with ZrB2 that embodiment 2 obtains, and d is the slurry being dispersed with ZrB2 that embodiment 3 obtains.
As can be seen from Fig. 1 ~ 4, the dispersion effect of the inventive method is good, be uniformly dispersed, slurry obvious sediment can not occur by 24h.
The slurry being dispersed with ZrB2 obtained embodiment 1 ~ 6 carries out the test of grain diameter measurement and Zeta potential, shown in its result table 1.
Table 1
The Zeta potential absolute value > 35mv of slurry, illustrates that intergranular space resistance can make slurry form stable suspension.The agglomerate size < 300nm of particle in the slurry, illustrates that the reunion degree of nano particle is lower, can form stable suspension in 24h.

Claims (10)

1. the method for dispersing nanometer ZrB2 powder, is characterized in that the method, carries out according to the following steps:
One, obtain by acidometric titration deionized water the solvent that pH is 3;
Two, take ZrB2 powder and dispersant, successively join in solvent by ZrB2 powder and dispersant, ultrasonic 14 ~ 16min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
2. the method for dispersing nanometer ZrB2 powder according to claim 1, is characterized in that in step one, acid is lactic acid.
3. the method for dispersing nanometer ZrB2 powder according to claim 1 and 2, it is characterized in that the average grain diameter of ZrB2 powder in step 2 is 100nm, purity is greater than 99%.
4. the method for dispersing nanometer ZrB2 powder according to claim 3, is characterized in that in step 2, dispersant is polymine.
5. the method for dispersing nanometer ZrB2 powder according to claim 4, it is characterized in that the quality of ZrB2 powder in step 2 is 2% of solvent quality, the quality of dispersant is 2% ~ 6% of ZrB2 powder quality.
6. the method for dispersing nanometer ZrB2 powder, carry out according to the following steps:
One, obtain by alkalimetric titration deionized water the solvent that pH is 11;
Two, take ZrB2 powder and dispersant, successively join in solvent by ZrB2 powder and dispersant, ultrasonic 14 ~ 16min, obtains finely dispersed slurry, namely completes the dispersion of nanometer ZrB2 powder.
7. the method for dispersing nanometer ZrB2 powder according to claim 6, is characterized in that in step one, alkali is ammoniacal liquor.
8. the method for the dispersing nanometer ZrB2 powder according to claim 6 or 7, it is characterized in that the average grain diameter of ZrB2 powder in step 2 is 100nm, purity is greater than 99%.
9. the method for dispersing nanometer ZrB2 powder according to claim 8, is characterized in that in step 2, dispersant is ammonium polyacrylate.
10. the method for dispersing nanometer ZrB2 powder according to claim 9, it is characterized in that the quality of ZrB2 powder in step 2 is 2% of solvent quality, the quality of dispersant is 2% ~ 6% of ZrB2 powder quality.
CN201410631888.9A 2014-11-11 2014-11-11 Dispersing method for ZrB2 nanopowder Pending CN104437155A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106854287A (en) * 2016-12-20 2017-06-16 华南理工大学 A kind of method for disperseing nanocrystalline cellulose powder in an aqueous medium

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CN1394918A (en) * 2001-07-06 2003-02-05 韩巍 Nano Water dispersion medium composition, its preparation method and application
US20090048087A1 (en) * 2006-05-22 2009-02-19 Zhang Shi C High-density pressurelessly sintered zirconium diboride/silicon carbide composite bodies and a method for producing the same
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106854287A (en) * 2016-12-20 2017-06-16 华南理工大学 A kind of method for disperseing nanocrystalline cellulose powder in an aqueous medium
CN106854287B (en) * 2016-12-20 2019-07-16 华南理工大学 A method of dispersing nanocrystalline cellulose powder in an aqueous medium

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