CN104458517B - The method for measuring flake metal powder radius-thickness ratio - Google Patents
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Abstract
The present invention relates to a kind of method for measuring flake metal powder radius-thickness ratio, including：Step one：The supporting body with end plane is made using powder is inlayed；Step 2：The suspension containing flake metal powder is coated with the end plane of supporting body, the metal-powder is dispersed in liquid dispersant and forms the suspension；Step 3：After after dispersant volatilization, powder will be inlayed to being added on end plane；Step 4：Make supporting body and inlay powder one entirety of formation；Step 5：Overall incision is formed through the incision face of end plane with perpendicular to the direction of end plane；Step 6：The length-width ratio of the cross section of the multiple flake metal powders on measurement incision face, thus obtains the radius-thickness ratio of flake metal powder.The method according to the invention, can easily measure flake metal powder radius-thickness ratio, and the precision of resulting radius-thickness ratio is higher.
Description
Technical field
The present invention relates to metal material field, more particularly to a kind of method for measuring flake metal powder radius-thickness ratio.
Background technology
Flake metal powder is widely used in coating, electronic component, and the radius-thickness ratio of flake metal powder is
Its important parameter that can be used.
In the prior art, radius-thickness ratio is measured usually using following methods：
(1) indivedual flake metal powders for erecting are searched under electron microscope, and uses electron microscope or optics
It is measured microscopically its radius-thickness ratio.But the flake metal powder erect is seldom, and lookup is extremely difficult, and resulting data also compare
It is unilateral, it is difficult to react the global feature of flake metal powder.
(2) using the optical microscope measuring measured with Z axis disperse the thickness of flake metal powder in the plane and
Length, by calculating radius-thickness ratio.Due to not being to be in close contact between flake metal powder and plane, but between there are
Gap, therefore radius-thickness ratio obtained by causing has larger deviation.
Accordingly, it would be desirable to need the method for improving the radius-thickness ratio for measuring flake metal powder.
The content of the invention
Regarding to the issue above, the present invention proposes a kind of method for measuring flake metal powder radius-thickness ratio.According to the present invention
Method, can easily measure flake metal powder radius-thickness ratio, and the precision of resulting radius-thickness ratio is higher.
The method of measurement flake metal powder radius-thickness ratio of the invention, including, step one：Tool is made using powder is inlayed
There is the supporting body of end plane；Step 2：The suspension containing flake metal powder, piece are coated with the end plane of supporting body
Shape metal-powder is dispersed in liquid dispersant and forms the suspension；Step 3：After dispersant volatilizees, will be to end plane
Powder is inlayed in upper addition；Step 4：Make supporting body and inlay powder one entirety of formation；Step 5：With perpendicular to the side of end plane
Formed through the incision face of end plane to this is integrally cut；Step 6：Multiple flake metal powders on measurement incision face
The length-width ratio of the cross section of body, thus obtains the radius-thickness ratio of flake metal powder.
The method according to the invention, flake metal powder knows from experience the end plane that there is supporting body in the way of horizontal parallel
On, it can be seen that the cross section of these flake metal powders exists in the way of horizontal parallel so on incision face.Parallel presence
Flake metal powder enable to the length-width ratio for measuring cross section to become very convenient such that it is able to it is very convenient and exactly
Measure the radius-thickness ratio of these flake metal powders.Additionally, the flake metal powder of parallel presence also allows for intuitively comparing sheet
The radius-thickness ratio of metal, so as to can just not obtain the substantially pattern of flake metal powder by carefully measurement.
In one embodiment, the length-width ratio in step 6 is multiplied by the correction factor k more than 1, to obtain sheet metal
Radius-thickness ratio after the optimization of powder.It is in irregular shape due to flake metal powder, but thickness is more uniform, therefore often not
The maximum gauge of flake metal powder can be measured on incision face and causes measured length-width ratio or radius-thickness ratio less than normal.Thus,
After measured length-width ratio or radius-thickness ratio are multiplied by into the correction factor k more than 1, the footpath of flake metal powder can be more realistically reacted
Thickness rate.
In one embodiment, correction factor k is obtained by following steps：Step a：Flake metal powder is laid in flat
On face, the maximum gauge of the multiple flake metal powders of measurement, and calculate the arithmetic average L of measured multiple maximum gauges；
Step b：The flake metal powder come in process step a using above-mentioned step one to five, the multiple flake metal powders of measurement
Cross-section lengths, and calculate the arithmetic average l of measured multiple cross-section lengths；Step c：Correction factor k is flat to count
The ratio of average L and arithmetic average l.Process is obtained from correction factor k, it comprises the maximum of flake metal powder
The factor of diameter, therefore after measured length-width ratio or radius-thickness ratio are multiplied by into the correction factor k more than 1, can more realistically react
The radius-thickness ratio of flake metal powder.Further, since the process for obtaining correction factor k is not related to measure flake metal powder completely
Thickness, therefore correction factor k can more accurately react sheet metal also not comprising the error of the thickness of flake metal powder is related to
The property of powder.
In one embodiment, in step 6, incision face is made metallographic flour milling, flake metal powder is then measured again
Cross section length-width ratio.After metallographic is prepared, the cross section of flake metal powder can significantly distinguish with supporting body, and this has
Help accurately measure the length-width ratio of flake metal powder.
In one embodiment, in step 2, dispersant is polar solvent.Polar solvent can well soak sheet
Metal-powder, so that flake metal powder can thoroughly scatter in the polarity dispersant, rather than reunion together.By
This, after dispersant is vapored away, these flake metal powders can just be stacked in parallel with each other, to facilitate measurement.
In a preferred embodiment, the dispersant also includes the non-polar solven dissolved each other with polar solvent.So, it is non-
Polarity can soak the flake metal powder that can not be soaked by polar solvent, so that all types of metal-powders can be
It is thoroughly dispersed out in dispersant.Preferably, non-polar solven and the mol ratio of polar solvent are 9:1 to 5:5.
In a specific embodiment, polar solvent is ethanol, non-polar solven is ether.Ether can not only be soaked not
Can be by the flake metal powder of ethanol wet, additionally it is possible to reduce the usage amount of ethanol.Due to can more or less contain water in ethanol
Point, these moisture can influence the precision of measurement result, and adding ether can reduce the usage amount of ethanol, so as to also just reduce
Water in dispersant, and then it is favorably improved the precision of measurement result.
In one embodiment, powder is inlayed for resin.In a specific embodiment, the resin is Lauxite or phenol
Urea formaldehyde.The melt temperature of resin is relatively low such that it is able to multiple supporting bodies are formed as into an entirety in the way of hot pressing, and
Help to carry out follow-up cutting operation.
It should be noted that, the step in present specification is not specific, and user can be according to actual conditions to this
A little steps are adjusted.
Compared with prior art, the advantage of the invention is that：(1) the method according to the invention, can be seen on incision face
The cross section of flake metal powder exists in the way of horizontal parallel, and the flake metal powder of parallel presence causes to measure cross section
Length-width ratio become very convenient such that it is able to radius-thickness ratio that is very convenient and measuring these flake metal powders exactly.(2)
The flake metal powder of parallel distribution also allows for intuitively comparing the radius-thickness ratio of sheet metal, so that not by carefully measurement with regard to energy
Access the substantially pattern of flake metal powder.
Brief description of the drawings
The invention will be described in more detail below based on embodiments and refering to the accompanying drawings.Wherein：
The step of Fig. 1 schematically shows implementation the method according to the invention schematic diagram.
Fig. 2 schematically shows the light microscope metallograph of the first embodiment according to the inventive method.
Fig. 3 shows the radius-thickness ratio distribution of the flake metal powder measured according to the first embodiment of the inventive method
Figure.
Fig. 4 schematically shows the light microscope metallograph of the second embodiment according to the inventive method.
Fig. 5 shows the radius-thickness ratio distribution of the flake metal powder measured according to the second embodiment of the inventive method
Figure.
Fig. 6 schematically shows the light microscope metallograph of the 3rd embodiment according to the inventive method.
Fig. 7 shows the radius-thickness ratio distribution of the flake metal powder measured according to the 3rd embodiment of the inventive method
Figure.
Specific embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
As shown in figure 1, carrying out step 11 first：Supporting body is prepared using powder is inlayed.Then, step 12 is carried out：Preparation contains
There is the suspension of flaky metal powder, and be applied on supporting body.Then, step 13 is carried out：After treating that dispersant volatilization is finished,
Powder is inlayed to being sprinkled on the end face, and forms pressed compact.Then, step 14 is carried out：Pressed compact is carried out into hot pressing and is made mosaic block.That is,
Form an entirety.Then, step 15 is carried out：Cut mosaic block.Finally, step 16 is carried out：Lamellar gold on measurement incision face
Belong to the length-width ratio of the cross section of powder, thus obtain the radius-thickness ratio of flake metal powder.
Embodiment 1：
Step one：Make cylindrical carrier body as powder is inlayed using Lauxite (that is, electricity beautiful), and by supporting body
Two end faces are made plane.
Step 2：Prepare dispersant：0.1 mole of ethanol and 0.8 mole of ether are uniformly mixed.By flaked tantalum powder 15
Gram it is put into prepared dispersant, and it is dispersed into suspension.Suspension is uniformly applied to carrying using dropper
On one end face of body.
Step 3：After treating that dispersant volatilization is finished, powder is inlayed to being sprinkled on the end face, and by supporting body and inlay powder
It is pressed into pressed compact (that is, forming an entirety).Preferably, the end of pressed compact can be made plane, and in an identical manner
To being coated with suspension in the plane, sprinkling and inlay powder, then suppress again.It is highly preferred that can prepare comprising 3 to 5 layers of tantalum powder
Pressed compact.
Step 4：Pressed compact is carried out into hot pressing and is made mosaic block.
Step 5：Formed through the incision face of end face with cutting mosaic block perpendicular to the direction of end face.Then, will cut
The face of opening is made metallographic flour milling.
Step 6：Use the length and width of the flaked tantalum powder cross section on electron microscope or optical microscope measuring metallographic flour milling
Than, and carry out rounding.
Fig. 2 shows a captured metallograph, and wherein reference 1 indicates the cross section of flaked tantalum powder.From
Be can be seen in Fig. 2, the cross section general parallel orientation of flaked tantalum powder.Table 1 shows the length and width of the cross section of measured flaked tantalum powder
The distribution of ratio.
Next correction factor k is obtained.First, by tantalum powder tiling mentioned above in the plane, multiple tantalum powders are measured
Maximum gauge, and it is 13.5 microns to calculate the arithmetic average L of measured multiple maximum gauges.Use above-mentioned steps one to five
The tantalum powder, the cross-section lengths of the multiple tantalum powders of measurement are processed again, and it is flat to calculate counting for measured multiple cross-section lengths
Average l is 10.6 microns.Correction factor k is the ratio of arithmetic average L and arithmetic average l, as 1.27.
Length-width ratio in table 1 is multiplied by into 1.27, and (that is, correction factor k), obtains the radius-thickness ratio of tantalum powder, as shown in table 2.Fig. 3
The ratio shared by the tantalum powder of different radius-thickness ratios is shown in the way of distribution curve.
Table 1
| Aspect ratio range | Quantity | Ratio |
| 0~2 | 5 | 2% |
| 2~4 | 48 | 21% |
| 4~6 | 45 | 20% |
| 6~8 | 48 | 21% |
| 8~10 | 27 | 12% |
| 10~12 | 29 | 13% |
| 12~14 | 18 | 8% |
| 14~16 | 4 | 2% |
| 16~18 | 1 | 0% |
| 18~20 | 1 | 0% |
| 20~22 | 4 | 2% |
| >=22 | 0 | 0% |
| Sum | 230 | 100% |
Table 2
| Ratio is classified | Number | Ratio |
| 0~2 | 2 | 1% |
| 2~4 | 24 | 10% |
| 4~6 | 42 | 18% |
| 6~8 | 36 | 16% |
| 8~10 | 38 | 17% |
| 10~12 | 22 | 10% |
| 12~14 | 26 | 11% |
| 14~16 | 21 | 9% |
| 16~18 | 9 | 4% |
| 18~20 | 4 | 2% |
| 20~22 | 1 | 0% |
| >=22 | 5 | 2% |
| Sum | 230 | 100% |
| Average value | 9.3 |
Embodiment 2：
The experimentation of embodiment 2 is same as Example 1, repeats no more here.The difference is that only：Rubbed using 0.3
Your ethanol and 0.7 mole of ether uniformly mixing and be made dispersant, then 20 grams of tantalum powders are put into prepared
It is in dispersant and dispersed into suspension.
Fig. 4 shows a captured metallograph, and wherein reference 3 indicates the cross section of flaked tantalum powder.From
Be can be seen in Fig. 4, the cross section general parallel orientation of flaked tantalum powder.Table 3 shows the length and width of the cross section of measured flaked tantalum powder
The distribution of ratio.
The value of resulting correction factor k is 1.27.Length-width ratio in table 3 is multiplied by into 1.27, and (that is, correction factor k), obtains
To the radius-thickness ratio of tantalum powder, as shown in table 4.Fig. 5 shows the ratio shared by the tantalum powder of different radius-thickness ratios in the way of distribution curve.
Table 3
| Ratio is classified | Number | Ratio |
| 0~2 | 5 | 2% |
| 2~4 | 38 | 16% |
| 4~6 | 51 | 22% |
| 6~8 | 55 | 23% |
| 8~10 | 23 | 10% |
| 10~12 | 34 | 14% |
| 12~14 | 18 | 8% |
| 14~16 | 5 | 2% |
| 16~18 | 2 | 1% |
| 18~20 | 0 | 0% |
| 20~22 | 5 | 2% |
| >=22 | 1 | 0% |
| Sum | 237 | 100% |
Table 4
| Ratio is classified | Number | Ratio |
| 0~2 | 2 | 1% |
| 2~4 | 18 | 8% |
| 4~6 | 44 | 19% |
| 6~8 | 36 | 15% |
| 8~10 | 48 | 20% |
| 10~12 | 17 | 7% |
| 12~14 | 33 | 14% |
| 14~16 | 15 | 6% |
| 16~18 | 11 | 5% |
| 18~20 | 4 | 2% |
| 20~22 | 3 | 1% |
| >=22 | 6 | 3% |
| 237 | 100% | |
| Average value | 9.6 |
Embodiment 3：
The experimentation of embodiment 3 is same as Example 1, repeats no more here.The difference is that only：Rubbed using 0.2
Your ethanol and 0.8 mole of ether uniformly mixing and be made dispersant, then 20 grams of tantalum powders are put into prepared
It is in dispersant and dispersed into suspension.
Fig. 6 shows a captured metallograph, and wherein reference 5 indicates the cross section of flaked tantalum powder.From
Be can be seen in Fig. 6, the cross section general parallel orientation of flaked tantalum powder.Table 5 shows the length and width of the cross section of measured flaked tantalum powder
The distribution of ratio.
The value of resulting correction factor k is 1.27.Length-width ratio in table 5 is multiplied by into 1.27, and (that is, correction factor k), obtains
To the radius-thickness ratio of tantalum powder, as shown in table 6.Fig. 7 shows the ratio shared by the tantalum powder of different radius-thickness ratios in the way of distribution curve.
Table 5
| Ratio is classified | Number | Ratio |
| 0~2 | 6 | 3% |
| 2~4 | 25 | 11% |
| 4~6 | 58 | 25% |
| 6~8 | 43 | 18% |
| 8~10 | 30 | 13% |
| 10~12 | 25 | 11% |
| 12~14 | 14 | 6% |
| 14~16 | 22 | 9% |
| 16~18 | 7 | 3% |
| 18~20 | 1 | 0% |
| 20~22 | 0 | 0% |
| >=22 | 2 | 1% |
| Sum | 233 | 100% |
Table 6
| Ratio is classified | Number | Ratio |
| 0~2 | 0 | 0% |
| 2~4 | 16 | 7% |
| 4~6 | 34 | 15% |
| 6~8 | 47 | 20% |
| 8~10 | 34 | 15% |
| 10~12 | 21 | 9% |
| 12~14 | 22 | 9% |
| 14~16 | 17 | 7% |
| 16~18 | 13 | 6% |
| 18~20 | 17 | 7% |
| 20~22 | 7 | 3% |
| >=22 | 5 | 2% |
| Sum | 233 | 100% |
| Average value | 10.5 |
Using method of the prior art, " optical microscope measuring with Z axis measurement disperses lamellar gold in the plane
Belong to the thickness and length of powder, by calculating radius-thickness ratio " measure used in embodiment 1, embodiment 2 and embodiment 3
Tantalum powder average aspect ratio, as a result as shown in table 7.
Known in those skilled in the art：For piece shape tantalum powder, radius-thickness ratio average value is bigger, then specific surface area is got over
Greatly.Here the specific surface area of the tantalum powder used in embodiment 1, embodiment 2 and embodiment 3 is also measured, as a result such as the institute of table 7
Show.
Table 7
Be can obtain from table 7：The specific surface area of the tantalum powder used in embodiment 1, embodiment 2 and embodiment 3 is gradually
It is increased.The radius-thickness ratio average value of the tantalum powder in embodiment 1, embodiment 2 and embodiment 3 is measured using the method according to the invention
It is also gradually increased, and the radius-thickness ratio average value of the tantalum powder measured using the method for prior art is not gradually increased.It is special
It is not the tantalum powder used for embodiment 2 and embodiment 3, the average value for measuring radius-thickness ratio using the method for prior art is phase
Together.This explanation method of the present invention can more accurately measure the radius-thickness ratio of flaky metal powder.
Although by reference to preferred embodiment, invention has been described, is not departing from the situation of the scope of the present invention
Under, various improvement can be carried out to it.The every technical characteristic being previously mentioned in each embodiment can have been combined in any way
Come.The invention is not limited in specific embodiment disclosed herein, but all skills including falling within the scope of the appended claims
Art scheme.
Claims (9)
1. it is a kind of measure flake metal powder radius-thickness ratio method, including：
Step one：The supporting body with end plane is made using powder is inlayed；
Step 2：Suspension of the coating containing the flake metal powder, the sheet on the end plane of the supporting body
Metal-powder is dispersed in liquid dispersant and forms the suspension；
Step 3：After after dispersant volatilization, powder is inlayed to being added on the end plane；
Step 4：The supporting body and the powder of inlaying is set to form an entirety；
Step 5：The overall incision is formed through the incision face of end plane with perpendicular to the direction of end plane；
Step 6：The length-width ratio of the cross section of multiple flake metal powders on the incision face is measured, described is thus obtained
The radius-thickness ratio of shape metal-powder.
2. method according to claim 1, it is characterised in that the length-width ratio in step 6 is multiplied by the amendment system more than 1
Number k, with the radius-thickness ratio after the optimization for obtaining the flake metal powder.
3. method according to claim 2, it is characterised in that the correction factor k is obtained by following steps：
Step a：By flake metal powder tiling in the plane, the maximum gauge of the multiple flake metal powders of measurement, and count
Calculate the arithmetic average L of measured multiple maximum gauges；
Step b：The step of usage right requirement 1 one to five, processes the flake metal powder in the step a, the multiple pieces of measurement
The cross-section lengths of shape metal-powder, and calculate the arithmetic average l of measured multiple cross-section lengths；
Step c：The correction factor k is the ratio of arithmetic average L and arithmetic average l.
4. the method according to any one of Claim 1-3, it is characterised in that in the step 6, by the incision
Face is made metallographic flour milling, and the length-width ratio of the cross section of flake metal powder is then measured again.
5. the method according to any one of Claim 1-3, it is characterised in that in the step 2, dispersant is pole
The mixture of property solvent and non-polar solven, and the polar solvent dissolves each other with the non-polar solven.
6. method according to claim 5, it is characterised in that the non-polar solven is 9 with the mol ratio of polar solvent:
1 to 5:5.
7. method according to claim 6, it is characterised in that the polar solvent is that ethanol, the non-polar solven are
Ether.
8. the method according to any one of Claim 1-3, it is characterised in that the powder of inlaying is for resin.
9. method according to claim 8, it is characterised in that the resin is Lauxite or phenolic resin.
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| CN110186738B (en) * | 2018-02-22 | 2021-11-02 | 宁波新材料测试评价中心有限公司 | Preparation method of flaky powder section sample |
| CN110261278A (en) * | 2019-07-11 | 2019-09-20 | 宁波石墨烯创新中心有限公司 | A method of measurement grapheme material powder specific-surface area detection |
| CN114235649A (en) * | 2021-12-20 | 2022-03-25 | 珠海真理光学仪器有限公司 | Particle diameter-thickness ratio measuring method and device based on laser particle sizer and storage medium |
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