CN102445461A - Method for detecting uniformity of powder injection molded feed - Google Patents
Method for detecting uniformity of powder injection molded feed Download PDFInfo
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- CN102445461A CN102445461A CN2011103063441A CN201110306344A CN102445461A CN 102445461 A CN102445461 A CN 102445461A CN 2011103063441 A CN2011103063441 A CN 2011103063441A CN 201110306344 A CN201110306344 A CN 201110306344A CN 102445461 A CN102445461 A CN 102445461A
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Abstract
The present invention discloses a method for detecting uniformity of a powder injection molded feed. The method comprises: selecting a material requiring detection; carrying out sampling for the material requiring detection; observing the sample by a scanning electron microscope (SEM); partitioning the obtained SEM pictures; adopting an image processing software to carry out statistics for the partitioned region; grouping the statistical results, and processing the grouped data to obtain the uniformity index. The method of the present invention has characteristics of simple process, convenient operation and short time consuming. With the method of the present invention, the uniformity of the powder injection molded feed can be high-precisionly and quantitatively detected on the microscopic state. The method is applicable for detection of the uniformity of the powder injection molded feed.
Description
Technical field
The invention discloses the inhomogeneity detection method of a kind of powder injection forming feeding.
Background technology
Powder injection forming is on the basis of prior powder metallurgy technology; An emerging near-net-shape technology that has creatively combined the injection molding technology of plastics industry and grown up; Having conventional powder metallurgy and the incomparable advantage of machine-tooled method aspect the manufacturing high-quality precision component, in national economy, obtained increasing application.The basic craft course of powder injection forming comprises: powder is evenly mixed with organic binder bond, be shaped with injection machine, then the cementing agent in the shaping base is removed, after sintering densification obtains product.Wherein producing uniform feeding is one of precondition that obtains high precision powder injection forming product.Thereby feeding is inhomogeneous will to be caused product that uneven contraction takes place in the later stage sintering process having a strong impact on the precision of final products, even causes defectives such as cracking.Because the feeding homogeneity has great significance to the precision control and the yield rate of power injection molding, therefore need to set up and estimate the inhomogeneity method of feeding reliably.
At present, use in the commercial production that to estimate the inhomogeneity method of feeding the most widely be through measuring the variation of equipment moment of torsion in the batch mixing process.Adopt the theoretical foundation of the method to be: at the initial stage of batch mixing, because powder and cementing agent dispersion are inhomogeneous, a large amount of powder is still reunited together, and this moment, the moment of torsion of mixing equipment was very big, and changed more violent; After this along with the carrying out of batch mixing process; A large amount of powder of reuniting are distributed in the middle of the cementing agent, and the feeding homogeneity constantly is improved, and the moment of torsion of mixing equipment constantly reduces; When prolongation, when no longer changing, the equipment moment of torsion can think that this moment, feeding mixed fully along with the time.The inhomogeneity shortcoming that adopts the method to estimate feeding is; This method can only judge that evenly whether feeding from macroscopic view; The same batch of inhomogeneity quality of inner feeding can not be estimated, size stability between same batch of parts spare that inside produced and the part can't be guaranteed.
In addition, adopting the density from feeding different parts sampling measurement sample, estimate the feeding homogeneity according to the mean square deviation of gained sample rate, also is the inhomogeneity method of a kind of detection feeding.Its shortcoming is, when institute's sample thief volume was big, the method was the same with calibrated wrench method, can only be evenly whether from macroscopic view judgement feeding, and can not estimate the same batch of inhomogeneity quality of inner feeding; And institute's sample thief volume hour, and zones of different feeding density variation is little, measures accuracy and just reduces greatly.
ESEM can carry out microcosmic to material and detect, and therefore is widely used in the observation of the uniform microstructure property of some materials such as powder, parts section.But homogeneity for the powder injection forming feeding; But never detect with ESEM, its reason is, contains a large amount of cementing agents in the middle of the feeding; Cementing agent and powder mix mutually; If not through statistical method, be difficult to directly it judged, lack a quantitative basis for estimation.
Summary of the invention
Technical matters to be solved by this invention provide a kind of high precision, can be quantitative the inhomogeneity method of detection powder injection forming feeding, help the control of powder injection forming product precision.
In order to solve the problems of the technologies described above, the inhomogeneity method of detection powder injection forming feeding provided by the invention may further comprise the steps:
The first step: the selection of feeding and sampling:
Feeding is selected a kind of feeding that is mixed by powder and cementing agent, and at least two of feeding different position samples, the quality of sample is greater than 0.5g;
Second step: scanning electron microscopic observation:
To selected feeding sample preparation, place under the ESEM and observe, obtain the electromicroscopic photograph of diverse location feeding;
The 3rd step: the division of electromicroscopic photograph and mathematical statistics:
The zone that electromicroscopic photograph is divided into n homalographic; N is even number and n>=16, adopts image analysis software that the powder area percentage composition in each zone is added up, and the data result with statistics is equally divided into two groups then; The number of each group is n/2, bigger numerical value A
1, A
2, A
3 
Be divided into one group, than fractional value
A
nBe divided into another group, respectively two groups of data averaged, as follows:
Adopt feeding Evaluation for Uniformity index H to estimate the homogeneity of feeding:
H=Δ μ=1-(μ
Greatly-μ
Little) formula 3
H between 0 to 1, when feeding fully evenly the time, this moment μ
Greatly=μ
Little, H equals 1; When feeding does not mix fully, this moment μ
GreatlyEqual 1, μ
LittleEqual 0, H equals 0; Along with the inhomogeneity raising of feeding, μ
GreatlyAnd μ
LittleBetween difference reduce gradually, the H value increases; It is better that evenness index surpasses 0.8 o'clock this regional feeding homogeneity, is suitable for powder injection forming.
Feeding of the present invention is selected a kind of by the feeding of powder with the cementing agent mixing, and described feeding is that powder is a kind of in stainless steel, low alloy steel, titanium alloy, the tungsten-molybdenum alloy; Cementing agent is one or more in stearic acid, vegetable oil, paraffin, tygon, polypropylene, polymethacrylate, the polyglycol, and the powder charging capacity of feeding is 55-70% (percent by volume).
The said image processing software that powder area percentage composition is added up comprises Image-Pro Plus, Leica QWin, a kind of among the NIH Image etc.
Adopt the inhomogeneity method of detection powder injection forming feeding of technique scheme,, obtain feeding Evaluation for Uniformity index based on ESEM and mathematical statistics.For estimating microscopic uniformity with the zones of different of a collection of feeding, select 2 above different parts to take a sample, to selected feeding sample preparation, place under the ESEM and observe, obtain the photo of different parts feeding; Electromicroscopic photograph is divided into the zone of at least 16 homalographics, guarantees that measurement result is accurate; Whether adopt image analysis software that the powder area percentage composition in each zone is added up, the data result with statistics is equally divided into two groups then, and two groups of data are averaged, adopt feeding Evaluation for Uniformity index assessment feeding even.The division of sampling among the present invention, scanning electron microscopic observation, electromicroscopic photograph and mathematical statistics are crucial, and whether the number of main consideration sampling is enough to represent feeding, thereby the whole homogeneity of feeding is estimated.The division number of electromicroscopic photograph needs more than 16 at least, to improve the precision of statistics.Whether the data result of statistics is equally divided into two groups, two groups of data are averaged, it is even to obtain feeding Evaluation for Uniformity index assessment feeding.
In above-mentioned technological process, influence the representativeness that is mainly sampling, observes of feeding Evaluation for Uniformity index, divide the number of photo.Take a sample through selecting 2 above different parts; The quality of sample is more than 0.5g; The feeding that can guarantee different parts in same batch obtains to detect; Electromicroscopic photograph is divided into the zone of 16 above homalographics, adopts image analysis software that the powder area percentage composition in each zone is added up, can guarantee the precision that homogeneity is calculated.
In sum; The inventive method technology is simple; Weak point easy to operate, consuming time; Division and mathematical statistics through sampling, scanning electron microscopic observation, electromicroscopic photograph are estimated the homogeneity of feeding, can be from high precision on the microcosmic, quantitative detection powder injection forming feeding homogeneity, and the homogeneity that is suitable for the powder injection forming feeding detects.
Description of drawings
Fig. 1 is 17-4PH stainless steel feeding position 1 place's stereoscan photograph;
Fig. 2 is 17-4PH stainless steel feeding position 2 place's stereoscan photographs;
Fig. 3 is 17-4PH stainless steel feeding stereoscan photograph position 1 place's zoning plan;
Fig. 4 is 17-4PH stainless steel feeding stereoscan photograph position 2 place's zoning plans;
Fig. 5 is Ti-6Al-4V feeding position 1 place's stereoscan photograph;
Fig. 6 is Ti-6Al-4V feeding position 2 place's stereoscan photographs;
Fig. 7 is Ti-6Al-4V feeding stereoscan photograph position 1 place's zoning plan;
Fig. 8 is Ti-6Al-4V feeding stereoscan photograph position 2 place's zoning plans.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further.
The inhomogeneity microcosmic detection method of powder injection forming feeding provided by the invention may further comprise the steps:
The first step: the selection of feeding:
Feeding is selected a kind of feeding that is mixed by metal powder and cementing agent, and metal powder is stainless steel, low alloy steel, titanium alloy, tungsten-molybdenum alloy or tungsten-cobalt carbide wimet; Cementing agent is one or more in stearic acid, paraffin, tygon, polypropylene, polymethacrylate and the polyglycol, and at least two of feeding different position samples, the quality of sample is greater than 0.5g;
Second step: scanning electron microscopic observation:
To selected feeding sample preparation, place under the ESEM and observe, obtain the electromicroscopic photograph of different parts feeding;
The 3rd step: the division of electromicroscopic photograph and mathematical statistics:
Electromicroscopic photograph is divided into the zone of N homalographic, and N is even number and N >=16, adopts image analysis software that the powder area percentage composition in each zone is added up; Data result with statistics is equally divided into two groups then; The number of each group is N/2, bigger numerical value A1, A2, A3 ... An/2 is divided into one group, than fractional value An/2+1, An/2+2, An/2+3 ... An is divided into another group; Respectively two groups of data are averaged, as follows:
μ
Greatly=2 (A1+A2+ ... + An/2)/n formula 1
μ
Little=2 (An/2+1+An/2+2+An/2+3 ... + An)/n formula 2
Adopt feeding Evaluation for Uniformity index H to estimate the homogeneity of feeding:
H=Δ μ=1-(μ
Greatly-μ
Little), formula 3
H between 0 to 1, when feeding fully evenly the time, this moment μ
Greatly=μ
Little, H equals 1; When feeding does not mix fully, this moment μ
GreatlyEqual 1, μ
LittleEqual 0, H equals 0; Along with the inhomogeneity raising of feeding, μ
GreatlyAnd μ
LittleBetween difference reduce gradually, the H value increases; Therefore, feeding homogeneity Factor H is big more, and then the feeding homogeneity is high more; Feeding homogeneity Factor H thinks that greater than 0.8 o'clock this regional feeding has good uniformity.
Powder area percentage composition is added up said image processing software comprise Image-Pro Plus, Leica QWin, a kind of among the NIH Image etc.
Embodiment 1:
Select 17-4PH stainless steel feeding, the powder charging capacity of feeding is 55% (percent by volume), and cementing agent is a stearic acid 5%, paraffin 35%, polymethacrylate 25%, tygon 35%, choose 2 diverse locations each 0.5g of feeding, sample preparation.Put into ESEM then and observe, it is as depicted in figs. 1 and 2 to obtain photo.It is carried out area dividing, be divided into 16 parts that area equates according to table 1, like Fig. 3 and shown in Figure 4.Utilize Image-Pro Plus software that 16 zones are added up again.The order acquisition result who presses table 1 is following: the statistics of position 1 electromicroscopic photograph: 72.3%, 71.2%, 55.3%, 52.2%, 65.5%, 57.8%; 78.4%, 81.3%, 57.2%, 51.7%, 51.3%; 79.2%, 73.1%, 85.3%, 54.3%, 55.6%; The statistics of position 2 electromicroscopic photographs: 52.5%, 58.6%, 61.2%, 60.9%, 59.9%, 53.5%, 55.6%, 55.8%, 60.5%, 68.5%, 52.6%, 50.2%, 51.6%, 58.6%, 56.8%, 61.3%.The statistics of position 1,2 electromicroscopic photographs is divided into groups respectively, like table 2, shown in 3.To big group with group in statistics average respectively, calculate its evenness index and be respectively: 0.786 and 0.924.Prove that this feeding is not good in the homogeneity in zone 1, and having good uniformity of zone 2 explained to exist in this feeding and mixed uneven zone.
Table 1 feeding stereoscan photograph is divided table
| A1 | A2 | A3 | A4 |
| A5 | A6 | A7 | A8 |
| A9 | A10 | A11 | A12 |
| A13 | A14 | A15 | A16 |
The grouping situation of table 2 position 1 place's statistics
| Greatly | Little |
| 85.30％ | 57.8％ |
| 81.30％ | 57.2％ |
| 79.20％ | 55.6％ |
| 78.40％ | 55.3％ |
| 73.10％ | 54.3％ |
| 72.30％ | 52.2％ |
| 71.20％ | 51.7％ |
| 65.50％ | 51.3％ |
The grouping situation of table 3 position 2 place's statisticss
| Greatly | Little |
| 68.5％ | 56.8％ |
| 61.3％ | 55.8％ |
| 61.2％ | 55.6％ |
| 60.9％ | 53.5％ |
| 60.5％ | 52.6％ |
| 59.9％ | 52.5％ |
| 58.6％ | 51.6％ |
| 58.6％ | 50.2％ |
Embodiment 2:
Select the Ti-6A1-4V feeding, binder system is a stearic acid 10%, vegetable oil 25%, polymethacrylate 30%, polypropylene 35%,, the powder charging capacity of feeding is 70% (percent by volume), choose 2 diverse locations each 1g of feeding, sample preparation.Put into ESEM then and observe, obtain photo such as Fig. 5 and shown in Figure 6.It is carried out area dividing, be divided into 16 parts that area equates according to table 1, like Fig. 7 and shown in Figure 8.Utilize Leica QWin software that 16 zones are added up again.The acquisition result is following: the statistics of position 1 electromicroscopic photograph: 76.3%, 65.2%, 59.3%, 61.2%, 69.4%, 74.6%, 71.3%, 66.8%, 81.5%, 83.5%, 90.2%, 52.1%, 73.4%, 79.3%, 66.3%, 73.6%; The statistics of position 2 electromicroscopic photographs: 78.5%, 72.6%, 83.4%, 86.5%, 56.6%, 75.2%, 78.6%, 65.3%, 88.5%, 75.8%, 64.7%, 75.9%, 81.6%, 78.3%, 74.1%, 76.7%.The statistics of position 1,2 electromicroscopic photographs is divided into groups respectively, like table 4, shown in 5.To big group with group in statistics average respectively, calculate its evenness index and be respectively: 0.849 and 0.885.Prove that this feeding is all good with the homogeneity in zone 2 in zone 1, explain not exist in this feeding and mix uneven zone.
The grouping situation of table 4 position 1 place's statistics
| Greatly | Little |
| 90.2％ | 71.3％ |
| 83.5％ | 69.4％ |
| 81.5％ | 66.8％ |
| 79.3％ | 66.3％ |
| 76.3％ | 65.2％ |
| 74.6％ | 61.2％ |
| 73.6％ | 59.3％ |
| 73.4％ | 52.1％ |
The grouping situation of table 5 position 2 place's statisticss
| Greatly | Little |
| 88.5％ | 75.9％ |
| 86.5％ | 75.8％ |
| 83.4％ | 75.2％ |
| 81.6％ | 74.1％ |
| 78.6％ | 72.6％ |
| 78.5％ | 65.3％ |
| 78.3％ | 64.7％ |
| 76.7％ | 56.6％ |
Embodiment 3:
Select the 93W-4Ni-3Fe feeding, binder system is a stearic acid 5%, polyglycol 15%, polymethacrylate 40%, tygon 40%,, the powder charging capacity of feeding is 60% (percent by volume), choose 3 diverse locations each 3g of feeding, sample preparation.Putting into ESEM then observes.It is carried out area dividing, be divided into 16 parts that area equates according to table 1.Utilize NIH Image software that 16 zones are added up again.The acquisition result is following: the statistics of position 1 electromicroscopic photograph: 66.1%, 61.4%, 59.6%, 92.5%, 86.4%, 62.5%, 50.6%, 53.4%, 54.6%, 37.3%, 74.6%, 79.2%, 49.3%, 58.5%, 62.1%, 68.2%; The statistics of position 2 electromicroscopic photographs: 45.4%, 76.2%, 62.2%, 68.4%, 57.5%, 73.1%, 81.2%, 83.5%, 79.3%, 50.1%, 56.5%, 59.1%, 65.7%, 78.3%, 80.2%, 33.9%; The statistics of position 3 electromicroscopic photographs: 65.4%, 86.1%, 64.5%, 38.7%, 77.2%, 70.2%, 51.3%, 64.5%, 59.4%, 39.1%, 67.2%, 69.3%, 63.2%, 78.4%, 75.1%, 63.6%.The statistics of position 1,2,3 electromicroscopic photographs is divided into groups respectively, like table 6,7, shown in 8.To big group with group in statistics average respectively, calculate its evenness index and be respectively: 0.791,0.763 and 0.819.Prove that this feeding is all not good with the homogeneity in zone 2 in zone 1, zone 3 has good uniformity, and explains to exist many places to mix uneven zone in this feeding.
The grouping situation of table 6 position 1 place's statistics
| Greatly | Little |
| 92.5 | 61.4 |
| 86.4 | 59.6 |
| 79.2 | 58.5 |
| 74.6 | 54.6 |
| 68.2 | 53.4 |
| 66.1 | 50.6 |
| 62.5 | 49.3 |
| 62.1 | 37.2 |
The grouping situation of table 7 position 2 place's statisticss
| Greatly | Little |
| 83.5 | 65.7 |
| 81.2 | 62.2 |
| 80.2 | 59.1 |
| 79.3 | 57.5 |
| 78.3 | 56.5 |
| 76.2 | 50.1 |
| 73.1 | 45.4 |
| 68.4 | 33.9 |
The grouping situation of table 8 position 3 place's statisticss
| Greatly | Little |
| 86.1 | 64.5 |
| 78.4 | 64.5 |
| 77.2 | 63.6 |
| 75.1 | 63.2 |
| 70.2 | 59.4 |
| 69.3 | 51.3 |
| 67.2 | 39.1 |
| 65.4 | 38.7 |
Claims (6)
1. one kind is detected the inhomogeneity method of powder injection forming feeding, it is characterized in that: may further comprise the steps:
The first step: the selection of feeding and sampling:
Feeding is selected a kind of feeding that is used for the powder injection forming test or produces that is mixed with by powder and cementing agent, at least two of feeding different position samples;
Second step: scanning electron microscopic observation:
To selected feeding sample preparation, place under the ESEM and observe, obtain the electromicroscopic photograph of diverse location feeding;
The 3rd step: the division of electromicroscopic photograph and mathematical statistics:
The zone that electromicroscopic photograph is divided into n homalographic; N is even number and n>=16, adopts image analysis software that the powder area percentage composition in each zone is added up, and the data result with statistics is equally divided into two groups then; The number of each group is n/2, bigger numerical value A
1, A
2, A
3 Be divided into one group, than fractional value
A
nBe divided into another group, respectively two groups of data averaged, as follows:
Adopt feeding Evaluation for Uniformity index H to estimate the homogeneity of feeding:
H=Δ μ=1-(μ
Greatly-μ
Little) formula 3
It is better that evenness index surpasses 0.8 o'clock this regional feeding homogeneity, is suitable for powder injection forming.
2. the inhomogeneity method of detection powder injection forming feeding according to claim 1; It is characterized in that: described feeding is selected a kind of by the feeding of powder with the cementing agent mixing, and described powder is a kind of in stainless steel, low alloy steel, titanium alloy, the tungsten-molybdenum alloy.
3. the inhomogeneity method of detection powder injection forming feeding according to claim 1 and 2; It is characterized in that: described feeding is selected a kind of feeding that is mixed by powder and cementing agent, and cementing agent is one or more in stearic acid, vegetable oil, paraffin, tygon, polypropylene, polymethacrylate, the polyglycol.
4. the inhomogeneity method of detection powder injection forming feeding according to claim 1 and 2 is characterized in that: the powder charging capacity percent by volume of feeding is 55-70%.
5. the inhomogeneity method of detection powder injection forming feeding according to claim 1 and 2 is characterized in that: get the feeding sample quality greater than 0.5g.
6. the inhomogeneity method of detection powder injection forming feeding according to claim 1 and 2 is characterized in that: powder area percentage composition is added up said image processing software comprise Image-Pro Plus, Leica QWin, a kind of among the NIH Image.
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Cited By (2)
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| CN106404701A (en) * | 2016-08-31 | 2017-02-15 | 上海交通大学 | Method for rapidly detecting mixing uniformity of protein in polymer solution |
| CN117074451A (en) * | 2023-10-12 | 2023-11-17 | 天津力神电池股份有限公司 | Method for detecting distribution state of prelithiation material in pole piece |
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| CN1196144C (en) * | 2000-05-29 | 2005-04-06 | 大同特殊钢株式会社 | Isotropic powdery magnetic material, preparation thereof and resin binded magnet |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106404701A (en) * | 2016-08-31 | 2017-02-15 | 上海交通大学 | Method for rapidly detecting mixing uniformity of protein in polymer solution |
| CN117074451A (en) * | 2023-10-12 | 2023-11-17 | 天津力神电池股份有限公司 | Method for detecting distribution state of prelithiation material in pole piece |
| CN117074451B (en) * | 2023-10-12 | 2024-01-12 | 天津力神电池股份有限公司 | Method for detecting distribution state of prelithiation material in pole piece |
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