CN101769847A - Method for measuring average grain size and particle size distribution of polytetrafluoroethylene powder - Google Patents
Method for measuring average grain size and particle size distribution of polytetrafluoroethylene powder Download PDFInfo
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- CN101769847A CN101769847A CN201010002837A CN201010002837A CN101769847A CN 101769847 A CN101769847 A CN 101769847A CN 201010002837 A CN201010002837 A CN 201010002837A CN 201010002837 A CN201010002837 A CN 201010002837A CN 101769847 A CN101769847 A CN 101769847A
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Abstract
The invention provides a method for measuring the average grain size (D50, namely medium diameter) and particle size distribution of polytetrafluoroethylene powder. The method of the invention comprises the following two methods: 1. cleanser essence/isopropanol is used as infiltrating system, water is used as dispersing medium, a laser granulometer is used to measure the average grain size and particle size distribution of polytetrafluoroethylene powder in the disperse system, the method is applicable to the measurement of average grain size of 2mu m-300mu m of polytetrafluoroethylene powder; and 2. compressed gas is used as dispersing medium, the dispersing pressure is controlled to 0.4-1.0bar, the laser granulometer is used to measure the average grain size and particle size distribution of polytetrafluoroethylene powder in the disperse system, and the method is applicable to the measurement of average grain size of 200mu m-1000mu m of polytetrafluoroethylene powder. The method of the invention can be used to convenient, fast and stably measure the average grain size and particle size distribution of polytetrafluoroethylene powder and is applicable to the measurement of average grain size of 2mu m-1000mu m of polytetrafluoroethylene powder.
Description
Technical field
The present invention relates to a kind of method of measuring the polytetrafluoroethylpowder powder mean grain size, specifically, relate to a kind of method of utilizing laser particle analyzer to measure polytetrafluoroethylpowder powder mean grain size and size distribution thereof.
Background technology
It is new developing technology in recent years that laser method test powder granularity distributes, and spreads to fields such as scientific research, production gradually.The laser particle analyzer of its use is integrated laser technology, modern optical power technology, electronic technology, precision optical machinery and computer technology have quick, the advantages such as dynamic range is big, easy and simple to handle, good reproducibility of test.
Teflon is described as " plastics king ", it is the high molecular polymer that is formed by the tetrafluoroethene homopolymerization, having excellent chemical stability, sealing, high lubricated not viscosity, electrical insulating property and good ageing resistance, is one of material of known decay resistance the best.It is widely used in the industrial circles such as atomic energy, national defence, space flight, electronics, electric, chemical industry, machinery, instrument, instrument, building, weaving, Treatment of Metal Surface, pharmacy, medical treatment, weaving, food, metallurgical smelting.The teflon relative molecular weight is bigger, is generally millions ofly, and the crystalline region fusing point is 327 ℃, has the molecular structure of rigidity, and melt viscosity is up to 10
10PaS, so it can not be with the method moulding of general thermoplastics.The polytetrafluoroethylpowder powder material often adopts the powder metallurgic method moulding, and sintering temperature can not surpass 410 ℃ at 360～375 ℃, also can adopt cold-extruded to go out the processes or the extrusion molding of sintering again.In forming process, outside the Pass product quality was removed and to be had with internal factors such as the mean molecular weight of polytetrafluoroethylpowder powder material, crystalline structure, crystallinity, the mean grain size of powder body material and size distribution also can produce material impact to the teflon product.Flowability, the venting quality of polytetrafluoroethylpowder powder material in process all has than big-difference, and therefore on market, mean grain size (D50 claims meso-position radius again) has become an important indicator weighing the polytetrafluoroethylpowder powder material.Seek accurately, intuitively, the method mean grain size and the size distribution that characterize the polytetrafluoroethylpowder powder material becomes problem demanding prompt solution efficiently.
In the existing ASTM D4894 standard, adopt the mean grain size and the distribution thereof of screen net spraying method test polytetrafluoroethylpowder powder material, the organic reagent that uses is zellon, and certain chemical toxicity is arranged; Also adopt among the HG/T 2901 and use the same method, but changed organic reagent into ethanol.Screen net spraying method test period is long, and the result is not directly perceived, and has used organic reagent in a large number, and long-term contact has certain harmfulness to operating personnel.Classify standard method of test as though laser method is measured the particle diameter of polytetrafluoroethylpowder powder material among the ISO 12086-2, concrete test process is not set forth.Though the report of laser method test polytetrafluoroethylfine fine particle mould pressing powder is arranged in the existing document, and its test specification is narrow, ethanol is general to the teflon wellability in the practical operation, and dispersion effect is poor in water, and the test peak shape lacks normal distribution.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing laser particle analyzer easily and fast, stably to measure polytetrafluoroethylpowder powder mean grain size (D50 claims meso-position radius again) and size distribution thereof.
In order to realize the object of the invention, a kind of method of measuring polytetrafluoroethylpowder powder mean grain size and size distribution thereof of the present invention, it is to be the infiltration system with liquid detergent and isopropyl alcohol, with water is dispersion medium, mean grain size and size distribution thereof with polytetrafluoroethylpowder powder in the laser particle analyzer wet method annex measurement dispersed system are suitable for the measurement of the polytetrafluoroethylpowder powder mean grain size of 2 μ m-300 μ m.
The mass ratio of liquid detergent and isopropyl alcohol is 1: 5～15 in the aforesaid method, wherein infiltration system.
Mass ratio according to 1: 5～10 in polytetrafluoroethylpowder powder adds above-mentioned infiltration system, mixes, and leaves standstill then more than 3 minutes; Add together in the dispersion medium water soaking into good polytetrafluoroethylpowder powder and infiltration system, the concentration of polytetrafluoroethylpowder powder in dispersion medium water is 0.1～1.0wt%, behind rotating speed 1000～3000rpm stirring 30s, measure the mean grain size of polytetrafluoroethylpowder powder in the dispersed system with laser particle analyzer wet method annex.
The liquid detergent that adopts among the present invention is commercially available, as goldfish board liquid detergent, white cat board liquid detergent etc.
In order to realize the object of the invention, the another kind of method of measuring polytetrafluoroethylpowder powder mean grain size and size distribution thereof of the present invention, it is to be dispersion medium with the pressure gas, mean grain size and size distribution thereof with polytetrafluoroethylpowder powder in the laser particle analyzer dry method annex measurement dispersed system are suitable for the measurement of the polytetrafluoroethylpowder powder mean grain size of 200 μ m-1000 μ m.
Aforesaid method, the dispersive pressure of wherein said pressure gas are 0.4～1.0bar.
Aforesaid method, wherein said pressure gas is selected from one or more in the gases such as air, nitrogen, helium.
By technique scheme, the present invention has following advantage and beneficial effect at least:
(1) adopts method of the present invention can easily and fast, stably measure the mean grain size and the size distribution thereof of polytetrafluoroethylpowder powder, be suitable for the measurement of 2 μ m-1000 μ m polytetrafluoroethylpowder powder mean grain sizes.
(2) the present invention uses liquid detergent and isopropyl alcohol to be the infiltration system, and its effect of impregnation may to polytetrafluoroethylpowder powder obviously is better than organic reagents such as ethanol, and test size distribution figure is normal distribution, good reproducibility.
(3) liquid detergent and the isopropyl alcohol of the present invention's use are cheap and easy to get, and consumption is few, and cost is low, and environmental pollution is little.
Description of drawings
Fig. 1 measures the mean grain size and the size distribution figure thereof of polytetrafluoroethylpowder powder micro mist in the dispersed system for laser particle analyzer wet method annex of the present invention;
Fig. 2 measures fine-grained mean grain size of polytetrafluoroethylpowder powder and size distribution figure thereof in the dispersed system for laser particle analyzer wet method annex of the present invention;
Fig. 3 is the mean grain size and the size distribution figure thereof of granularity 1 in the polytetrafluoroethylpowder powder in the laser particle analyzer wet method annex measurement dispersed system of the present invention;
Fig. 4 is the mean grain size and the size distribution figure thereof of granularity 2 in the polytetrafluoroethylpowder powder in the laser particle analyzer wet method annex measurement dispersed system of the present invention;
Fig. 5 is mean grain size and the size distribution figure thereof that laser particle analyzer wet method annex is measured polytetrafluoroethylpowder powder micro mist in the dispersed system;
Fig. 6 is that laser particle analyzer wet method annex is measured in the dispersed system mean grain size and the size distribution figure thereof of granularity 2 in the polytetrafluoroethylpowder powder;
Fig. 7 measures the mean grain size and the size distribution figure thereof of polytetrafluoroethylpowder powder in the dispersed system for laser particle analyzer dry method annex of the present invention;
Fig. 8 is mean grain size and the size distribution figure thereof that laser particle analyzer dry method annex is measured polytetrafluoroethylpowder powder in the dispersed system;
Fig. 9 tests trend map for D50 with dispersive pressure.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Mass ratio preparation liquid detergent and isopropyl alcohol by 1: 10 soak into system, and liquid detergent is evenly dispersed in the isopropyl alcohol.
Take by weighing ptfe micropowder to be measured, fine granularity, middle granularity 1, each 1g of middle granularity 2 samples respectively in the 25ml beaker, every kind of powder takes by weighing 5 parallel sample, in sample, add the liquid detergent and the isopropyl alcohol that prepare respectively and soak into system 8.0g, after mixing with the sample spoon, left standstill 3 minutes.In the sample cell of the HYDRO2000MU type wet method annex of Ma Erwen MASTERSIZER 2000 type laser particle analyzers, add 500ml water, the adjusting speed of agitator is 2200rpm, background correction, add in the sample cell soaking into good polytetrafluoroethylpowder powder, treat sample in sample cell, be uniformly dispersed (about 30 seconds), hit testing and logging test results, test result is as shown in table 1.
Table 1 testing sample D50 test result (the infiltration system is liquid detergent and isopropyl alcohol)
The infiltration system that Comparative Examples is prepared by 1: 10 mass ratio with NP-12 and ethanol
Take by weighing ptfe micropowder to be measured, fine granularity, middle granularity 1, each 1g of middle granularity 2 samples respectively in the 25ml beaker, every kind of powder takes by weighing 5 parallel sample, add the NP-12/ ethanol for preparing respectively and soak into system 8.0g, after mixing with the sample spoon, left standstill 3 minutes.In the sample cell of the wet method annex of Ma Erwen MU2000 type laser particle analyzer, add 500ml water, the adjusting speed of agitator is 2200rpm, background correction, add in the sample cell soaking into good polytetrafluoroethylpowder powder, treat sample in sample cell, be uniformly dispersed (about 30 seconds), hit testing and logging test results, test result is as shown in table 2.
Table 2 testing sample D50 test result (the infiltration system is NP-12 and ethanol)
In the present embodiment, the actual value of ptfe micropowder D50 to be measured is 2～5 μ m, and the actual value of fine granularity D50 is 25～35 μ m, and the actual value of middle granularity 1D50 is 80～100 μ m, and the actual value of middle granularity 2D50 is 180～220 μ m.By the contrast of the data in table 1 and the table 2 as can be seen, adopt liquid detergent and isopropyl alcohol to soak into system, it is good that it detects data reappearance, swift to operate, ptfe micropowder, fine granularity, middle granularity all there is wellability preferably, can obtain dispersion effect preferably, size distribution figure as shown in Figures 1 to 4.And when adopting NP-12 and ethanol system to soak into, all can not obtain satisfied dispersion effect to ptfe micropowder, middle granularity, and depart from actual value, test data is disperseed during actual the test, powder has conglomeration in water, as shown in Figure 5 and Figure 6, can not obtain true and reliable test data.
Take by weighing 5g polytetrafluoroethylpowder powder sample to be measured CGF218, put into Ma Erwen laser particle analyzer SCIROCCO 2000 type dry method annexes, it is 0.8bar that the pressure gas dispersive pressure is set, sample injection time is 8s, even sample introduction, repeated test is 5 times according to the method described above, and the typical case tests size distribution figure as shown in Figure 7, result such as table 3.
Table 3 polytetrafluoroethylpowder powder sample to be measured D50 test result
| Sequence number | ??1 | ??2 | ??3 | ??4 | ??5 | Mean value | Relative standard deviation |
| ??CGF218??D50μm | ??638 | ??642 | ??641 | ??641 | ??637 | ??640 | ??0.6％ |
In the present embodiment, the actual value of the D50 of polytetrafluoroethylpowder powder CGF218 to be measured is between 600～660 μ m, and the relative standard deviation of 5 repeated experiments only is 0.6%, and test consuming time less than 2 minutes at every turn, the favorable reproducibility of proof this method, data are tested quick accurately and reliably.
Take by weighing 5g polytetrafluoroethylpowder powder sample to be measured CGF218 at every turn, put into Ma Erwen laser particle analyzer SCIROCCO 2000 type dry method annexes, the pressure gas dispersive pressure is set, and (with 0.0bar is starting point, each experiment increases progressively 0.2bar, finish during up to dispersive pressure for 1.6bar), sample injection time is 8s, evenly sample introduction, the results are shown in Table 4, D50 with the dispersive pressure changing trend diagram as shown in Figure 9.
Table 4 testing sample D50 is with the dispersive pressure test result
| Sequence number | ??1 | ??2 | ??3 | ??4 | ??5 | ??6 | ??7 | ??8 | ??9 |
| Dispersive pressure (bar) | ??0.0 | ??0.2 | ??0.4 | ??0.6 | ??0.8 | ??1.0 | ??1.2 | ??1.4 | ??1.6 |
| ??CGF218??D50μm | ??873 | ??744 | ??646 | ??632 | ??640 | ??621 | ??577 | ??501 | ??479 |
In the present embodiment, the actual value of the D50 of polytetrafluoroethylpowder powder CGF218 to be measured is between 600～660 μ m.By table 4 test result as can be known, when dispersive pressure was lower than 0.4bar, the relative actual value of test result was bigger than normal, and its main cause is that dispersive pressure is low excessively, the polytetrafluoroethylpowder powder particle can not be disperseed effectively; When dispersive pressure was higher than 1.0bar, the relative actual value of test result was less than normal, from size distribution Fig. 8 as can be seen, the powder granule of 100 μ m has appearred in the size distribution being lower than, proof is under excessive dispersive pressure, and powder granule is smashed by air-flow, so test result is less than normal.
The above results explanation is being dispersion medium with the pressure gas, when polytetrafluoroethylpowder powder is carried out the size distribution test, must strict control disperse gaseous tension in suitable scope, too high or too lowly all can not obtain real test result.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (7)
1. method of measuring polytetrafluoroethylpowder powder mean grain size and size distribution thereof, it is characterized in that, with liquid detergent and isopropyl alcohol is the infiltration system, is dispersion medium with water, measures the mean grain size and the size distribution thereof of polytetrafluoroethylpowder powder in the dispersed system with laser particle analyzer wet method annex.
2. the method for claim 1 is characterized in that, the mass ratio of liquid detergent and isopropyl alcohol is 1: 5～15 in the described infiltration system.
3. the method for claim 1 is characterized in that, the mass ratio according to 1: 5～10 in polytetrafluoroethylpowder powder adds the infiltration system.
4. the method for claim 1 is characterized in that, the concentration of polytetrafluoroethylpowder powder in dispersion medium water is 0.1～1.0wt%.
5. a method of measuring polytetrafluoroethylpowder powder mean grain size and size distribution thereof is characterized in that, is dispersion medium with the pressure gas, measures the mean grain size and the size distribution thereof of polytetrafluoroethylpowder powder in the dispersed system with laser particle analyzer dry method annex.
6. method as claimed in claim 5 is characterized in that, the dispersive pressure of wherein said pressure gas is 0.4～1.0bar.
7. as claim 5 or 6 described methods, it is characterized in that wherein said pressure gas is selected from one or more in air, nitrogen or the helium.
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| CN102890043A (en) * | 2012-09-13 | 2013-01-23 | 浙江轻机实业有限公司 | Method for analyzing granularity of easily soluble materials |
| CN103018143A (en) * | 2012-12-05 | 2013-04-03 | 平顶山易成新材料股份有限公司 | Detection method of particle size of silicon carbide micropowder |
| CN103411860A (en) * | 2013-08-13 | 2013-11-27 | 中国检验检疫科学研究院 | Powder average particle size determination method |
| CN103630471A (en) * | 2013-11-20 | 2014-03-12 | 江苏大学 | Method for measuring median particle diameter of particles in exhaust gas of diesel engine |
| CN103792167A (en) * | 2014-01-22 | 2014-05-14 | 西安航天化学动力厂 | Method for testing granularity of 12-14 mu m ammonium perchlorate |
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| CN102890043A (en) * | 2012-09-13 | 2013-01-23 | 浙江轻机实业有限公司 | Method for analyzing granularity of easily soluble materials |
| CN103018143A (en) * | 2012-12-05 | 2013-04-03 | 平顶山易成新材料股份有限公司 | Detection method of particle size of silicon carbide micropowder |
| CN103018143B (en) * | 2012-12-05 | 2015-04-01 | 平顶山易成新材料有限公司 | Detection method of particle size of silicon carbide micropowder |
| CN103411860A (en) * | 2013-08-13 | 2013-11-27 | 中国检验检疫科学研究院 | Powder average particle size determination method |
| CN103630471A (en) * | 2013-11-20 | 2014-03-12 | 江苏大学 | Method for measuring median particle diameter of particles in exhaust gas of diesel engine |
| CN103630471B (en) * | 2013-11-20 | 2015-10-28 | 江苏大学 | The measuring method of particle median particle diameter in a kind of diesel exhaust gas |
| CN103792167A (en) * | 2014-01-22 | 2014-05-14 | 西安航天化学动力厂 | Method for testing granularity of 12-14 mu m ammonium perchlorate |
| CN104568540B (en) * | 2014-12-24 | 2017-12-26 | 上海理工大学 | A kind of preparation method of the standard particle solid sample of wide size distribution |
| CN104568540A (en) * | 2014-12-24 | 2015-04-29 | 上海理工大学 | Preparation method for wide-size-distribution standard particle solid sample |
| CN104535603A (en) * | 2014-12-25 | 2015-04-22 | 光为绿色新能源股份有限公司 | Method for detecting silicon carbide quality |
| CN107121363A (en) * | 2017-03-22 | 2017-09-01 | 华南理工大学 | A kind of method of crystallization processes process particle size distribution prediction |
| CN107132162A (en) * | 2017-05-17 | 2017-09-05 | 东旭科技集团有限公司 | A kind of particle diameter of alkaline earth metal carbonate powder and the assay method of particle diameter distribution |
| CN111766184A (en) * | 2020-06-30 | 2020-10-13 | 吉林大学 | Method for measuring particle size distribution of titanium hydride powder compact |
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