CN110146405A - The measuring method of boron carbide mass fraction in a kind of aluminum-based boron carbide neutron absorber material - Google Patents
The measuring method of boron carbide mass fraction in a kind of aluminum-based boron carbide neutron absorber material Download PDFInfo
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- CN110146405A CN110146405A CN201910485485.0A CN201910485485A CN110146405A CN 110146405 A CN110146405 A CN 110146405A CN 201910485485 A CN201910485485 A CN 201910485485A CN 110146405 A CN110146405 A CN 110146405A
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Abstract
The present invention provides a kind of measuring methods of boron carbide mass fraction in aluminum-based boron carbide neutron absorber material, belong to chemical analysis technology field.The present invention can be completely dissolved the property of aluminium base part in aluminum-based boron carbide neutron absorber material using dust technology or dilute hydrochloric acid in a heated state, the remaining boron carbide of whole stabilised qualities be obtained by being centrifuged, drying, to calculate mass fraction shared by boron carbide.Embodiment the result shows that, measuring method provided by the invention can Accurate Determining go out the mass fraction of boron carbide in aluminum-based boron carbide neutron absorber material, test result accuracy rate is up to 99.8%.
Description
Technical field
The present invention relates to chemical analysis technology field, in particular to boron carbide in a kind of aluminum-based boron carbide neutron absorber material
The measuring method of mass fraction.
Background technique
Aluminum-based boron carbide neutron absorber material is one kind using aluminium powder and boron carbide powder as the shielding protection material of substrate, often
For in the neutron-absorbing in nuclear power field and spentnuclear fuel field.Aluminium powder and boron carbide powder in aluminum-based boron carbide neutron absorber material
The proportion speed of powder material directly affects the ability that its neutron absorbing screen covers.However, since boron carbide material is insoluble in acid
Characteristic is difficult to adopt conventional chemical analysis means and accurately measures its proportion score in aluminum-based boron carbide material, causes existing
Stage has no the measuring method of boron carbide mass fraction in aluminum-based boron carbide neutron absorber material, and people can not confirm that aluminium base is carbonized
The product quality of boron neutron absorber material.
Summary of the invention
In view of this, it is an object of that present invention to provide boron carbide mass fractions in a kind of aluminum-based boron carbide neutron absorber material
Measuring method.Measuring method provided by the invention is easily operated, can Accurate Determining go out aluminum-based boron carbide neutron absorber material
The mass fraction of middle boron carbide.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of measuring methods of boron carbide mass fraction in aluminum-based boron carbide neutron absorber material, including
Following steps:
(1) aluminum-based boron carbide neutron absorber material is placed in container, dust technology or dilute hydrochloric acid is added, stopped wait reacting
When, heating obtains being evaporated object after being evaporated；
(2) object that is evaporated successively is washed, is centrifuged and dried to constant weight, record constant weight solid and container gross mass
M1；
(3) operation that constant weight solid is repeated to step (1), (2), obtains second of constant weight solid and container gross mass M2；
(4) M is calculated1、M2Double difference, if double difference < 0.1%, with M1With M2Average value it is total as constant weight solid and container
Mass M；If double difference >=0.1%, second of constant weight solid is continued to the operation for repeating step (1), (2), until MnWith M(n-1)'s
Double difference < 0.1%, with MnWith M(n-1)Average value as constant weight solid and container gross mass M, wherein MnIndicate that n-th tests institute
Obtain constant weight solid and container gross mass, M(n-1)Indicate constant weight solid and container gross mass obtained by (n-1)th test, n be >=3 it is whole
Number；
(5) mass fraction of boron carbide in aluminum-based boron carbide neutron absorber material is calculated according to Formulas I:
In Formulas I,For the mass fraction of boron carbide；
M is constant weight solid and container gross mass, unit g；
m1For container mass, unit g；
M is aluminum-based boron carbide neutron absorber material quality, unit g.
Preferably, in the step (1) aluminum-based boron carbide neutron absorber material side length≤5mm.
Preferably, dust technology in the step (1), dilute hydrochloric acid mass concentration independently be 5~20%；The dust technology
Or dilute hydrochloric acid is added by several times, the number being added by several times is 2~10 times.
Preferably, the mass ratio of the volume of the dust technology or dilute hydrochloric acid and aluminum-based boron carbide neutron absorber material is independently
For (20~200mL): 1g.
Preferably, the temperature that heating is evaporated in the step (1) is 90~100 DEG C.
Preferably, washing with detergent is secondary distilled water in the step (2).
Preferably, the revolving speed being centrifuged in the step (2) is 3000~4000r/min, time 30min.
Preferably, temperature dry in the step (2) is 105 ± 1 DEG C.
The present invention provides a kind of measuring methods of boron carbide mass fraction in aluminum-based boron carbide neutron absorber material.This hair
It is bright to be completely dissolved aluminium base part in aluminum-based boron carbide neutron absorber material in a heated state using dust technology or dilute hydrochloric acid
Property obtains the remaining boron carbide of whole stabilised qualities by being centrifuged, drying, to calculate quality shared by boron carbide point
Number.Embodiment the result shows that, measuring method provided by the invention can Accurate Determining go out in aluminum-based boron carbide neutron absorber material
The mass fraction of boron carbide, test result accuracy rate is up to 99.8%.
Specific embodiment
The present invention provides a kind of measuring methods of boron carbide mass fraction in aluminum-based boron carbide neutron absorber material, including
Following steps:
(1) aluminum-based boron carbide neutron absorber material is placed in container, dust technology or dilute hydrochloric acid is added, stopped wait reacting
When, heating obtains being evaporated object after being evaporated；
(2) object that is evaporated successively is washed, is centrifuged and dried to constant weight, record constant weight solid and container gross mass
M1；
(3) operation that constant weight solid is repeated to step (1), (2), obtains second of constant weight solid and container gross mass M2；
(4) M is calculated1、M2Double difference, if double difference < 0.1%, with M1With M2Average value it is total as constant weight solid and container
Mass M；If double difference >=0.1%, second of constant weight solid is continued to the operation for repeating step (1), (2), until MnWith M(n-1)'s
Double difference < 0.1%, with MnWith M(n-1)Average value as constant weight solid and container gross mass M, wherein MnIndicate that n-th tests institute
Obtain constant weight solid and container gross mass, M(n-1)Indicate constant weight solid and container gross mass obtained by (n-1)th test, n be >=3 it is whole
Number；
(5) mass fraction of boron carbide in aluminum-based boron carbide neutron absorber material is calculated according to Formulas I:
In Formulas I,For the mass fraction of boron carbide；
M is constant weight solid and container gross mass, unit g；
m1For container mass, unit g；
M is aluminum-based boron carbide neutron absorber material quality, unit g.
Aluminum-based boron carbide neutron absorber material is placed in container by the present invention, and dust technology or dilute hydrochloric acid is added, stops wait react
When only, heating obtains being evaporated object after being evaporated.In the present invention, the aluminum-based boron carbide neutron absorber material side length preferably≤
5mm, more preferably≤3mm；The present invention does not have special requirement, this field to the source of the aluminum-based boron carbide neutron absorber material
Method of the invention can be used to be tested for conventional commercial or the aluminum-based boron carbide neutron absorber material voluntarily prepared.In this hair
In bright, the container is preferably glass centrifuge tube.The present invention will first hold preferably before aluminum-based boron carbide neutron absorber material is added
Device is dry to constant weight, and the temperature of the drying is preferably 105 DEG C.
In the present invention, the dust technology, dilute hydrochloric acid mass concentration be preferably independently 5~20%, more preferably 10
~15%；The dust technology or dilute hydrochloric acid are added by several times, and the number being added by several times is preferably 2~10 times；The dust technology is dilute
The volume of hydrochloric acid and the mass ratio of aluminum-based boron carbide neutron absorber material are independently preferably (20~200mL): 1g, more preferably
(50~150mL): 1g；In the present invention, the temperature being evaporated that heats is preferably 90~100 DEG C, and more preferably 94~98 DEG C；
The mode of the heating is preferably heating water bath；The time that the present invention is evaporated the heating does not have special requirement, can make
Solid is completely dried.The present invention is after being added dust technology or dilute hydrochloric acid, and aluminum-based boron carbide neutron is inhaled under the effect of heating
The aluminum material resolution received in material is aluminum nitrate or aluminium chloride, and boron carbide will not be cleared up.The present invention is by controlling dilute nitre
The temperature of the concentration and heating of acid or dilute hydrochloric acid, can aluminum material in rapid-digestion aluminum-based boron carbide neutron absorber material and
It can guarantee resolution completely, to obtain dry boron carbide powder.
It obtains after being evaporated object, the present invention successively washs, is centrifuged and dries to constant weight the object that is evaporated, and records constant weight
Solid and container gross mass M1.In the present invention, the washing is preferably secondary distilled water with detergent, the number of the washing
Preferably 2 times.The present invention can remove the aluminum nitrate or aluminium chloride in drying solid by washing.Present invention preferably uses from
Scheming is centrifuged, and the revolving speed of the centrifugation is preferably 3000~4000r/min, and the time is preferably 30min.The present invention by from
The heart can remove the impurity in remaining solid.
In the present invention, the temperature of the drying is preferably 105 DEG C；Present invention preferably uses baking ovens to be dried；It is described
It dries to constant weight method particularly includes: the solid after centrifugation is first put into 6~8h of oven drying, is then cooled to room temperature, is weighed；
Solid is put into baking oven again, 2h is dried at the same temperature, then cools to room temperature, is weighed；Repeat dry 2h, cooling and title
The operation of weight, until solid constant weight.
After obtaining constant weight solid, constant weight solid is repeated the operation of step (1), (2) by the present invention, and it is solid to obtain second of constant weight
Body and container gross mass M2.Calculate M1、M2Double difference, if double difference < 0.1%, with M1With M2Average value as constant weight solid and hold
Device gross mass M；If double difference >=0.1%, second of constant weight solid is continued to the operation for repeating step (1), (2), until MnWith
M(n-1)Double difference < 0.1%, with MnWith M(n-1)Average value as constant weight solid and container gross mass M, wherein MnIndicate n-th
Test gained constant weight solid and container gross mass, M(n-1)Indicate constant weight solid obtained by (n-1)th test and container gross mass, n is
>=3 integer.The present invention calculates the double difference according to Formula II:
Double difference=| Mn-M(n-1)The Formula II of |/m × 100%；
In Formula II, MnGained constant weight solid and container gross mass, unit g are tested for n-th；
M(n-1)For constant weight solid obtained by (n-1)th test and container gross mass, unit g；
M is aluminum-based boron carbide neutron absorber material quality, unit g.
After completing aforesaid operations, the present invention calculates the quality of boron carbide in aluminum-based boron carbide neutron absorber material according to Formulas I
Score:
In Formulas I,For the mass fraction of boron carbide；
M is constant weight solid and container gross mass, unit g；
m1For container mass, unit g；
M is aluminum-based boron carbide neutron absorber material quality, unit g.
In the present invention, describedCalculated result preferably retain to second after decimal point.
Below with reference to embodiment to boron carbide mass fraction in aluminum-based boron carbide neutron absorber material provided by the invention
Measuring method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Aluminum-based boron carbide neutron absorber material is prepared, raw material is boron carbide 25.5g, aluminium powder 74.5g.Preparation method packet
Include following steps:
(1) nuclear leve boron carbide powder and aluminium powder are uniformly mixed；
(2) by the mixed powder static pressure at embryo material；
(3) processing embryo material is machined to according to design requirement；
(4) processing embryo material surface anodization processing.
It is computed, the mass fraction of boron carbide is 25.5% in this aluminum-based boron carbide neutron absorber material.
Using this aluminum-based boron carbide neutron absorber material as raw material, aluminum-based boron carbide neutron-absorbing material provided by the invention is verified
The accuracy of boron carbide mass fraction measuring method in material.
(1) the aluminum-based boron carbide neutron absorber material (side length≤5mm) of precise 1.0030g, be placed in 105 DEG C it is dried
And to (quality is referred to as 34.1488g) in the 30mL glass centrifuge tube after constant weight, it is slowly added to the dust technology that mass concentration is 20%
Glass centrifuge tube is placed in 100 DEG C of water-bath and heats by 20mL, and 1~2 20mL dust technology is added when dry to the greatest extent, is proceeded to
After reactionless, it is evaporated to obtain drying solid；
(2) drying solid is washed 3 times using secondary distilled water, 30min is centrifuged using the centrifuge of 4000r/min later
6 hours dry, natural cooling is placed in 105 DEG C of baking ovens；Dry and cooling down operation is repeated later, until solid constant weight, at this time
Solid and glass centrifuge tube gross mass M1For 34.4042g；
(3) operation that constant weight solid is repeated to step (1), (2), obtains second of constant weight solid masses and container gross mass
M2For 34.4041g；Calculate M1、M2Double difference be 0.01%, this value < 0.1%, calculate M1、M2Average value be M=
34.4042g, using M as constant weight solid and container gross mass；
(4) content of boron carbide mass fraction is calculated according to Formulas I:
In Formulas I,For the mass fraction of boron carbide；
M is constant weight solid and container gross mass, unit g；
m1For container mass, unit g；
M is aluminum-based boron carbide neutron absorber material quality, unit g.
It is computed,Acquired results absolute measurement deviation is -0.04%, and test result accuracy rate is
99.8%.
Embodiment 2
Commercially available aluminum-based boron carbide neutron absorber material is bought, shows boron carbide mass fraction in this neutron absorber material ingredient
It is 31%.
Boron carbide mass fraction in this aluminum-based boron carbide neutron absorber material is measured using measuring method provided by the invention,
(1) precise 0.9688g aluminum-based boron carbide neutron absorber material (side length≤5mm), be placed in 105 DEG C it is dried simultaneously
In 30mL glass centrifuge tube after to constant weight (quality is referred to as 35.6435g), it is slowly added to the dilute hydrochloric acid that mass concentration is 10%
Glass centrifuge tube is placed in 95 DEG C of water-bath and heats by 20mL, and 2~3 20mL dilute hydrochloric acid are added when dry to the greatest extent, proceed to nothing
After reaction, it is evaporated to obtain drying solid；
(2) drying solid is washed 3 times using secondary distilled water, 30min is centrifuged using the centrifuge of 4000r/min later
8 hours dry, natural cooling is placed in 105 DEG C of baking ovens；Dry and cooling down operation is repeated later, until solid constant weight, at this time
Solid and glass centrifuge tube gross mass M1For 35.9446g；
(3) operation that constant weight solid is repeated to step (1), (2), obtains second of constant weight solid masses and container gross mass
M2For 35.9425g；Calculate M1、M2Double difference be 0.22%, this value > 0.1%, by second of constant weight solid continue repeat step
(1), the operation of (2), until MnWith M(n-1)Double difference < 0.1%, calculate MnWith M(n-1)Average value M=35.9425g, made with M
For constant weight solid and container gross mass；
(4) content of boron carbide mass fraction is calculated according to Formulas I:
In Formulas I,For the mass fraction of boron carbide；
M is constant weight solid and container gross mass, unit g；
m1For container mass, unit g；
M is aluminum-based boron carbide neutron absorber material quality, unit g.
It is computed,Acquired results absolute measurement deviation is -0.14%, and test result accuracy rate is
99.5%.
As can be seen from the above embodiments, measuring method provided by the invention can Accurate Determining go out aluminum-based boron carbide neutron-absorbing
The mass fraction of boron carbide in material.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. the measuring method of boron carbide mass fraction in a kind of aluminum-based boron carbide neutron absorber material, which is characterized in that including with
Lower step:
(1) aluminum-based boron carbide neutron absorber material is placed in container, dust technology is added or dilute hydrochloric acid adds when reacting stopping
Heat obtains being evaporated object after being evaporated；
(2) object that is evaporated successively is washed, is centrifuged and dried to constant weight, record constant weight solid and container gross mass M1；
(3) operation that constant weight solid is repeated to step (1), (2), obtains second of constant weight solid and container gross mass M2；
(4) M is calculated1、M2Double difference, if double difference < 0.1%, with M1With M2Average value as constant weight solid and container gross mass M；
If double difference >=0.1%, second of constant weight solid is continued to the operation for repeating step (1), (2), until MnWith M(n-1)Double difference <
0.1%, with MnWith M(n-1)Average value as constant weight solid and container gross mass M, wherein MnIndicate n-th test gained constant weight
Solid and container gross mass, M(n-1)Indicate constant weight solid obtained by (n-1)th test and container gross mass, the integer that n is >=3；
(5) mass fraction of boron carbide in aluminum-based boron carbide neutron absorber material is calculated according to Formulas I:
In Formulas I, ω(B4C)For the mass fraction of boron carbide；
M is constant weight solid and container gross mass, unit g；
m1For container mass, unit g；
M is aluminum-based boron carbide neutron absorber material quality, unit g.
2. measuring method according to claim 1, which is characterized in that aluminum-based boron carbide neutron-absorbing in the step (1)
Side length≤5mm of material.
3. measuring method according to claim 1, which is characterized in that the quality of dust technology, dilute hydrochloric acid in the step (1)
Concentration independently is 5~20%；The dust technology or dilute hydrochloric acid are added by several times, and the number being added by several times is 2~10 times.
4. measuring method according to claim 1 or 3, which is characterized in that the volume and aluminium of the dust technology or dilute hydrochloric acid
The mass ratio of base boron carbide neutron absorber material independently is (20~200mL): 1g.
5. measuring method according to claim 1, which is characterized in that the temperature that heating is evaporated in the step (1) is 90
~100 DEG C.
6. measuring method according to claim 1, which is characterized in that washing detergent is secondary in the step (2)
Distilled water.
7. measuring method according to claim 1, which is characterized in that the revolving speed being centrifuged in the step (2) is 3000~
4000r/min, time 30min.
8. measuring method according to claim 1, which is characterized in that dry temperature is 105 ± 1 in the step (2)
℃。
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2019
- 2019-06-05 CN CN201910485485.0A patent/CN110146405A/en active Pending
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