CN1420349A - Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing - Google Patents
Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing Download PDFInfo
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- CN1420349A CN1420349A CN02124156A CN02124156A CN1420349A CN 1420349 A CN1420349 A CN 1420349A CN 02124156 A CN02124156 A CN 02124156A CN 02124156 A CN02124156 A CN 02124156A CN 1420349 A CN1420349 A CN 1420349A
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Abstract
A process for preparing the specimen of chemically deposited nickel fixed alloy powder in order to observe it by transmission electron microscope includes preparing deposition solution in beaker, slowly putting the copper block coated with powder on an insulating plate in said solution, putting the beaker in water bath at 83-92 deg.C, chemical depositing for 4-6 hr, tearing the deposited film from the copper block, sticking it to frosted glass, abrasing to 30-50 microns by abrasive paper, punching to become small circular film with 3 mm of diameter, and ion thinning. Its advantages are easy control and high successful rate.
Description
Technical field:
The invention belongs to transmission electron microscope (TEM) laboratory sample preparing technical field.
Background technology:
Prepare in the alloy at powder metallurgy process, directly influence microstructure after the solid moulding of powder (hot and cold etc. static pressure etc.), thereby finally influence the mechanical property of material as the primitive powder particle solidified structure feature of alloy and phase composition meeting thereof.For optimizing flouring technology and selecting the subsequent machining technology parameter, usually need carry out systematic study to starting powder particle solidified structure feature, because powder particle tiny (tens microns between the hundreds of micron), make that the specimen preparation that is used for transmission electron microscope (TEM) observation is very difficult, perplex most of material structure researchers always, R.D.Field and H.L.Fraser and A.M.Ritter and M.EHenry once were fixed on the nickel base superalloy powder on the sheet copper with electro-plating method respectively in the literature, and make thin crystal, but the electro-plating method technological process is numerous and diverse, influence factor is more, success ratio is lower, cost is also expensive, adopts the chemical deposited nickel fixed alloy powder sample making technology also not appear in the newspapers and leads.
Summary of the invention:
The invention solves the electro-plating method technological process numerous and diverse,, success ratio is low,, problem such as cost height.
The present invention is by the design and analysis of utilization mathematical statistics orthogonal experiment, determine the stoicheiometry and the optimized parameters (temperature, time, powder quantity, pH value etc.) of optimum chemical nickel plating deposit fluid, alloy powder is fixed on chemical deposition on the copper billet of active state, obtains sedimentary deposit surface smoothing, compact and firm.Adopting special stripping means to strip down sedimentary deposit from copper billet becomes thin slice, makes metallographic observation sample and scanning electron microscope sample through suitable grinding, etch again, equally also can be used for the preparation of transmission electron microscope observing with thin crystal sample.
Technological process of the present invention is:
1, the proportioning of chemogenic deposit and experiment condition determines
Deposit fluid proportioning: nickelous sulfate: 24-26g/l+ inferior sodium phosphate: 22-23g/l+ anhydrous sodium acetate 14-1615g/l+ citric acid: 1.5-2.5g/l+ lead acetate: 2-3ml/l;
The deposit fluid pH value: 4.5～5 (use H
2SO
4Or NaOH adjusts);
Temperature: 83～92 ℃.
2, the fixing powder particle of chemical deposited nickel
Carry out fixedly powder particle of chemical deposited nickel with as shown in Figure 4 device, step is as follows:
(1) prepare deposit fluid by proportioning, treat that deposit fluid fully evenly after, check the pH value of deposit fluid with the PH test paper.
(2) brass ingot is polished flat with flint glass paper after, copper billet and powder are put into concentrated hydrochloric acid respectively activate 1～2 hour.
(3) use washed with de-ionized water respectively after the activation of copper billet and powder, and at once wetting powder is coated on the copper billet equably, and with clean glass sheet pressing, compacting.
(4) will put into the deposit fluid of 0.5-0.7 in the beaker, and put into a smooth insulating trip (as glass sheet etc.) that is a bit larger tham copper billet, the copper billet that will scribble powder is then put on the deposit fluid insulating trip gently.
(5) beaker is put into water bath with thermostatic control reposefully, bath temperature is adjusted to 83-92 ℃, carries out chemogenic deposit, will constantly add new deposit fluid in the deposition process, to guarantee deposition effect.
(6) deposition was taken out sample and water and is rinsed well after 4-6 hour, and chemogenic deposit finishes.
3, the preparation of the thin crystal style of powder particle
(1) film that will be deposited on the copper billet takes off, and sticks on the frosted glass again, and to 30-50 μ m, the sequin that is washed into diameter after taking off and is 3mm is used for ion milling with sand papering.
(2) vacuum tightness of ion thinning device is 10
-5-10
-4Pa, electric current 0.6-0.2mA, voltage 4.5-7KV, 5-10 hour attenuate time, ion beam angle 7-20 degree.Behind above-mentioned system attenuate, there is nearly central area, part powder particle edge thin district to occur, can be used for electronic microscope photos.
The invention has the advantages that: the chemical deposited nickel fixed alloy powder granule technology has that equipment is simple, easily-controlled operation, sample preparation success ratio advantages of higher.
Description of drawings
Fig. 1 is NiSO
4, NaH
2PO
2, NaAC content influences sedimentation velocity.Ordinate among the figure: sedimentation velocity (μ m/h); Horizontal ordinate: reagent content (%), curve 1 are that sodium acetate influences sedimentation velocity; Curve 2 is that inferior sodium phosphate influences sedimentation velocity; Curve 3 is that nickelous sulfate influences sedimentation velocity.
Fig. 2 is that citric acid content influences sedimentation velocity.Ordinate among the figure: sedimentation velocity (μ m/h); Horizontal ordinate: reagent content (%), curve 4 are that citric acid influences sedimentation velocity.
Fig. 3 coating and copper matrix bond shape appearance figure.Copper matrix 5, coating 6
Fig. 4 is a chemogenic deposit device synoptic diagram.Wherein electric-heated thermostatic water bath 7, switch 8, thermostatical pilot lamp 9, thermometer 10, beaker 11, deposit fluid 12, copper billet 13, glass sheet 14, alloy powder 15.
Fig. 5 is the thin crystal sample photo of successfully making of the present invention of TEM.Wherein
Embodiment:
1, the proportioning of chemogenic deposit and experiment condition determines
Prerun electroless nickel deposition formula of liquid and experiment condition are as follows:
Deposit fluid: nickelous sulfate (25g/l)+inferior sodium phosphate (22.5g/l)+anhydrous sodium acetate (15g/l)+citric acid (2g/l)+lead acetate (5/l);
Deposit fluid pH value: 4.6;
Experimental temperature: 88 ℃.
Substrate and powder: clean (30 minutes) with 5% hydrochloride alcohol solution, then even distribution nickel base powder high temperature alloy (FGH95) powder particle (Φ 50-150 μ m) on the copper billet of activation
In order to determine best proportioning deposit fluid, find out the rule that influences of each factor, adopt mathematical statistics orthogonal design and analysis, nickel sulfate content, ortho phosphorous acid sodium content, sodium acetate content, citric acid content a large amount of system experimentation researchs have been done to the influence of sedimentation velocity, shown in accompanying drawing 1, accompanying drawing 2, and carry out orthonormal design of experiments according to its data, and drawing best experimental program, its deposit fluid proportioning and experiment condition are as follows:
Deposit fluid proportioning: nickelous sulfate (25g/l)+inferior sodium phosphate (21g/l)+anhydrous sodium acetate (13.5g/l)+citric acid (2g/l)+lead acetate (2.5ml/l);
The solution pH value: 4.6 (use H
2SO
4Or NaOH adjusts);
Experimental temperature: 88 ℃.
Adopt above-mentioned deposit fluid proportioning and experiment condition, sedimentation velocity can reach 21 μ m/h, and sedimentary deposit surface smoothing, compact and firm are tight with powder particle and copper matrix bond, and Coating composition is Ni:91.159%, P:8.841% (Fig. 3).
2, the fixing powder particle technology of chemical deposited nickel
Carry out fixedly powder particle of chemical deposited nickel with as shown in Figure 4 device, step is as follows:
(1) prepare deposit fluid by proportioning, treat that deposit fluid fully evenly after, whether the pH value of checking deposit fluid with the PH test paper can be with the concentrated sulphuric acid or NaOH adjustment if any deviation between 4.5～5.
(2) with brass ingot (13 * 12mm) polish flat with flint glass paper (200#) after, copper billet and powder are put into concentrated hydrochloric acid activation 1.5 hours respectively.
(3) after the activation of copper billet and powder respectively for several times with washed with de-ionized water, and at once wetting powder is coated on the copper billet equably, and with clean glass sheet pressing, compacting.
(4) with the deposit fluid of putting into 0.6 in the beaker, and put into a smooth insulating trip (as glass sheet etc.) that is a bit larger tham copper billet, the copper billet that will scribble powder is then put on the deposit fluid insulating trip gently.
(5) beaker is put into water bath with thermostatic control reposefully, bath temperature is adjusted to 88 ℃, carries out chemogenic deposit, will constantly add new deposit fluid in the deposition process, to guarantee deposition effect.
(6) deposition was taken out sample and water and is rinsed well after 5 hours, and chemogenic deposit finishes.
3, the preparation of the thin crystal style of powder particle
(1) will deposit good sample and become metallographic specimen with sand papering after, sedimentary deposit is taken off from frosted glass, below sand papering to 50 μ m, the sequin that is washed into diameter and is 3mm is used for ion milling.
(2) (vacuum tightness is 10 the sequin of diameter 3mm to be put into LBS-1 ion thinning device
-5Pa), use wide-angle 20 degree (electric current 0.6mA, voltage 7KV) attenuates 5 hours earlier, spend (electric current 0.4mA, voltage 6KV) attenuates 10 hours with angle 14 again, spend (electric current 0.2mA, voltage 4.5KV) attenuates 7 hours with low-angle 7 then.Behind above-mentioned system attenuate, there is nearly central area, part powder particle edge thin district to occur, can be used for electronic microscope photos (Fig. 5 illustrates the transmission electron microscope photo for preparing sample with this method).
Claims (1)
1, a kind of method for making sample of chemical deposited nickel fixed alloy powder that is used for transmission electron microscope observing, it is characterized in that: technological process is:
Determining of the proportioning of a chemogenic deposit and experiment condition
Deposit fluid proportioning: nickelous sulfate: 24-26g/l+ inferior sodium phosphate: 22-23g/l+ anhydrous sodium acetate 14-1615g/l+ citric acid: 1.5-2.5g/l+ lead acetate: 2-3ml/l,
The deposit fluid pH value: 4.5-5,
Temperature: 83-92 ℃;
The b chemical deposited nickel is powder particle fixedly
Chemical deposited nickel is powder particle fixedly, and step is as follows: prepare deposit fluid by proportioning, treat that deposit fluid fully evenly after, check the pH value of deposit fluid with the PH test paper; After brass ingot polished flat with flint glass paper, copper billet and powder are put into concentrated hydrochloric acid activation 1-2 hour respectively; Use washed with de-ionized water respectively after the activation of copper billet and powder, and at once wetting powder is coated on the copper billet equably, and with clean glass sheet pressing, compacting; To put into the deposit fluid of 0.5-0.7 in the beaker, and put into a smooth insulating trip that is a bit larger tham copper billet, the copper billet that will scribble powder is then put on the deposit fluid insulating trip gently; Beaker is put into water bath with thermostatic control reposefully, and bath temperature is adjusted to 83-92 ℃, carries out chemogenic deposit, deposits after 4-6 hour, takes out sample and water and rinses well, and chemogenic deposit finishes;
The preparation of the thin crystal style of c powder particle
The film that is deposited on the copper billet is taken off, stick on the frosted glass again, to 30-50 μ m, the sequin that is washed into diameter after taking off and is 3mm is used for ion milling with sand papering.The vacuum tightness of ion thinning device is 10
-5-10
-4Pa, electric current 0.6-0.2mA, voltage 4.5-7KV, 5-10 hour attenuate time, ion beam angle 7-20 degree; Behind above-mentioned system attenuate, there is nearly central area, part powder particle edge thin district to occur, can be used for electronic microscope photos.
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Cited By (8)
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| CN102304748A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Preparation method of transmission electron microscope film sample through rapidly solidifying aluminum alloy powder |
| CN102841005A (en) * | 2012-09-20 | 2012-12-26 | 东南大学 | Preparation method for thin steel wire transmission electron microscope sample |
| CN103698178A (en) * | 2013-12-12 | 2014-04-02 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for thin-film sample for high-resolution transmission electron microscope |
| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN103868770A (en) * | 2014-02-24 | 2014-06-18 | 燕山大学 | Preparation method of granulate Fe-C compound transmission electron microscope in-situ tensile sample |
| CN107121316A (en) * | 2017-03-22 | 2017-09-01 | 华南理工大学 | A kind of preparation method of micron order Ni-base Superalloy Powder transmission electron microscope film sample |
| CN109030148A (en) * | 2018-07-27 | 2018-12-18 | 中南大学 | A kind of preparation method of iron(-)base powder EBSD detection sample |
| CN111239167A (en) * | 2020-02-19 | 2020-06-05 | 北京矿冶科技集团有限公司 | Preparation method of transmission electron microscope sample made of ultrafine powder material |
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2002
- 2002-07-12 CN CNB021241562A patent/CN1257396C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304748A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Preparation method of transmission electron microscope film sample through rapidly solidifying aluminum alloy powder |
| CN102304748B (en) * | 2011-09-14 | 2013-11-06 | 哈尔滨工业大学 | Preparation method of transmission electron microscope film sample through rapidly solidifying aluminum alloy powder |
| CN102841005A (en) * | 2012-09-20 | 2012-12-26 | 东南大学 | Preparation method for thin steel wire transmission electron microscope sample |
| CN103698178A (en) * | 2013-12-12 | 2014-04-02 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for thin-film sample for high-resolution transmission electron microscope |
| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN103868770A (en) * | 2014-02-24 | 2014-06-18 | 燕山大学 | Preparation method of granulate Fe-C compound transmission electron microscope in-situ tensile sample |
| CN103868770B (en) * | 2014-02-24 | 2016-08-24 | 燕山大学 | The preparation method of graininess Fe-C compound transmission electron microscope original position stretching sample |
| CN107121316A (en) * | 2017-03-22 | 2017-09-01 | 华南理工大学 | A kind of preparation method of micron order Ni-base Superalloy Powder transmission electron microscope film sample |
| CN109030148A (en) * | 2018-07-27 | 2018-12-18 | 中南大学 | A kind of preparation method of iron(-)base powder EBSD detection sample |
| WO2020019400A1 (en) * | 2018-07-27 | 2020-01-30 | 中南大学 | Preparation method for iron-based alloy powder ebsd test sample |
| CN109030148B (en) * | 2018-07-27 | 2020-09-29 | 中南大学 | Preparation method of iron-based alloy powder EBSD detection sample |
| CN111239167A (en) * | 2020-02-19 | 2020-06-05 | 北京矿冶科技集团有限公司 | Preparation method of transmission electron microscope sample made of ultrafine powder material |
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|---|---|
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