CN105738173B - A kind of preparation method of Material Wear section sample - Google Patents
A kind of preparation method of Material Wear section sample Download PDFInfo
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- CN105738173B CN105738173B CN201610104034.4A CN201610104034A CN105738173B CN 105738173 B CN105738173 B CN 105738173B CN 201610104034 A CN201610104034 A CN 201610104034A CN 105738173 B CN105738173 B CN 105738173B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- Analysing Materials By The Use Of Radiation (AREA)
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Abstract
The invention discloses a kind of preparation methods of Material Wear section sample, comprising the following steps: nickel-plating liquid is warming up to 50~80 DEG C, sample is placed in plating solution, stirs 30~50min of plating solution, obtains 0.5~2mm nickel plating protective layer；Wear specimens along perpendicular to rubbing surface, be parallel to glide direction and be cut into two parts, two parts sample is stacked, worn area is in contact and guarantees that two sections are parallel to each other and in the same side；Sample will be stacked and be put into embedding die, after fixation, casting metal conduction slurries, room temperature cooling into the gap of two wear surfaces；Sample carries out sand paper polishing, polishes and measure sample surfaces roughness Ra, and calculate the standard roughness of sample WhenWhen specimen surface roughness reach test request, carry out corrosion treatment.There is the present invention metal conductive fluid to replace inlaying resin, while guaranteeing solidification effect, the more conducively Electronic Speculum characterization of the characteristics such as abrasion section depth, pattern, and the advantage for simplifying preparation process further.
Description
Technical field
The present invention relates to a kind of preparation methods of Material Wear section sample, are more particularly applicable to Electronic Speculum
The preparation method of Material Wear section sample.
Background technique
After Material Wear, need to carry out table to its wear surface and sub-surface (perpendicular to the section of wear surface)
Sign to the characterization material degree of wear and discloses its friction since different tissues, pattern and performance is presented in sub-surface different depth
Wear mechanism has very great help, so that the design and application for friction material provide reference.
Good abrasion section sample is prepared, has highly important effect in metal material fretting wear research.It is made
Preparation Method is as follows: (1) sample clean: sample being cleaned by ultrasonic；(2) cut: Wear specimens are along perpendicular to rubbing surface, parallel
Sample is cut into two parts in glide direction；(3) it smears solidification glue: after metal-cured glue is smeared in worn area, two being ground
Damage face correspondence cements to form a sample；(4) inlay solidification: sample, which is put into, inlays mould, measures resin and curing agent according to the ratio, together
Section sample is made after the ambient temperature curing 20-40 of a certain amount of conductive nickel powder of Shi Tianjia；(5) sample grinding and polishing is handled: section sample
Carry out sand paper polishing, polishing and corrosion treatment.It has a problem in that 1, preparation method is more complex in preparation method at present, smears
Solidification glue is only to be convenient for being easy to hold in subsequent sample polishing treatment, and inlay in resin and add with cured effect is inlayed
Though entering nickel powder is easy to conductive, electric charge accumulation is easily caused to influence to characterize quality；2 but due to lacking enough worn areas
Protection, the mechanical damage of sample is larger, is easy to introduce deformation during the preparation process；Simultaneously because sample surfaces lack protection, edge
It is embedding the result is that edge effect polishing is undesirable, it is difficult to observation is clear；3, during sample grinding and buffing, often according to meat
The observation of eye and experience judge whether sample meets the requirements, and the sample often prepared in the case where lacking experience is not achieved wants
It asks, and needs to return again to laboratory and carry out sanding and polishing, often waste a large amount of time and efforts, on the whole, the prior art
Preparation method in mechanical lapping and polishing treatment quality it is lower, tissue and morphology characterization effect it is poor, sample is had damage.It is existing
Surface roughness is measured using instrument and equipment and tool in technology, sample is needed to take out from processing environment, it is very not square
Just time-consuming and laborious.
Summary of the invention
It is an object of the present invention to provide a kind of preparation methods of Material Wear section sample, use metal conductive fluid
Instead of inlaying resin, while guaranteeing solidification effect, convenient for observing the worn area of sample, the more conducively depth of research abrasion section
The characteristic of degree, pattern, and simplify preparation process further.
A further object of the invention is by summary of experience formula gauging surface roughness, for judging grinding and buffing mistake
Whether journey can reach sample testing requirements, save the time and improve sample preparation efficiency.
A further object of the invention carries out chemical plating to worn area surface, prevents that shape occurs during the preparation process
Become, enhances the protection to sample.
In order to realize these purposes and other advantages according to the present invention, a kind of Material Wear section sample is provided
Preparation method, comprising the following steps:
Step 1: nickel-plating liquid being warming up to 50~80 DEG C, sample is placed in plating solution, stirs 30~50min of plating solution, is obtained
0.5~2mm nickel plating protective layer；
Step 2: Wear specimens along perpendicular to rubbing surface, be parallel to glide direction and be cut into two parts, by two parts sample
It stacks, worn area is in contact and guarantees that two sections are parallel to each other and in the same side；
Step 3: sample will be stacked and be put into embedding die, after fixation, casting metal is conductive into the gap of two wear surfaces
Slurries, room temperature cooling；
Step 4: sample carries out sand paper polishing, polishes and measure sample surfaces roughness Ra, and the standard for calculating sample is thick
Rugosity
Wherein, A is the first impact factor；θ is grinding angle；H is the hardness of sample；R1、R2、R3It is followed successively by and beats for the first time
Mill, corase grinding, fine grinding sand paper partial size；α1、α2For constant；Κ is correction factor；
WhenWhen specimen surface roughness reach test request, carry out corrosion treatment.
Preferably, the sample of the step 1 first carries out 5~10min of ultrasonic cleaning.
Preferably, the surrounding of sample is fixed in the embedding die of the step 3.
Preferably, the embedding die is equipped with sprue gate.
Preferably, the metallic conduction slurries are conductive silver paste or conductive copper paste.
Preferably, the polishing in the step 4 and polishing direction with to casting area at 45 degree of angles.
Preferably, the polishing, which is divided into, polishes, roughly grinds and three step of fine grinding.
Preferably, the polishing is polished with the polished machine that revolving speed is 200-1200 revs/min.
Preferably, the corrosion treatment is to be cleaned and dried up with clear water with after etching solution etch.
The present invention is include at least the following beneficial effects:: 1, chemical nickel plating is carried out to sample worn area surface, prevents from cutting
It cuts, destroy worn area pattern during grinding and buffing.2, replaced inlaying resin with metal conductive fluid, not only simplify fall gluing this
One step, it is ensured that while inlaying effect, improve measurement accuracy.3, using formula gauging surface roughness, for judging to beat
Whether mill and polishing process can reach sample testing requirements, save the time and improve sample preparation efficiency.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
Fig. 1 is the cutting schematic diagram of Wear specimens of the invention.
Fig. 2 is the stacking diagram of two parts sample after cutting of the invention.
Fig. 3 is the structure chart stacked after sample fixation of the invention.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
Embodiment 1
A kind of preparation method of Material Wear section sample, comprising the following steps:
Pretreatment: being cleaned by ultrasonic 15-30 minutes with dehydrated alcohol, and acetone is cleaned by ultrasonic 10-20 minutes after drying, and drying is standby
With.
Step 1: chemical nickel plating.Nickel-plating liquid is warming up to 50-80 DEG C, the sample handled well is placed in plating solution, observation is
It is no to there is bubble to emerge, and it is stirred continuously plating solution.Plating 30min or more, thickness of coating reach 0.7mm；The plating piece that will have been plated later
It takes out, is eluted with water from plating solution, dry up；Nickel coating protects worn area, to guarantee that worn area is sent out in subsequent processing
Change shape.Wherein, the configuration proportion of nickel-plating liquid are as follows: nickel sulfate 25-35g/L, sodium hypophosphite 25-35g/L, sodium acetate 15-
25g/L, lactic acid 15-25g/L, 5~15mL/L of propionic acid, 90~140mg/L of Potassiumiodate, cetyl trimethylammonium bromide 50~
80mg/L。
Step 2: as shown in Figure 1, by Wear specimens along perpendicular to rubbing surface, be parallel to glide direction and be cut into two parts；
As shown in Fig. 2, two parts sample is symmetrically stacked, worn area is in contact and guarantees that two sections are parallel to each other and in the same side.
Step 3: sample will be stacked and be put into embedding die, sample is fixed in mold, from embedding die sprue gate to two
Sample is fixed in casting metal conductive silver paste, room temperature cooling, conductive silver paste in the gap of wear surface, is illustrated in figure 3 solid
The structure of sample after fixed, wherein the conductive layer 104 that conductive silver paste is formed connects upper layer and lower layer nickel coating 103, and two parts are tried
Sample is integrally fixed, and nickel coating protects worn area 102, and wherein the depth of worn area 102, pattern provide ginseng to research abrasion mechanism
It examines.
Step 4: sample carries out sand paper polishing, polishing.
Wherein, polishing, which is divided into, polishes, roughly grinds and three step of fine grinding, and the direction of polishing and casting area are in 45° angle.It polishes: using
600# silicon carbide paper, grinding angle are 45 degree, and the revolution of polished machine is set as 200~300 revs/min, and sample is made one and is put down
Face；Corase grinding: use 800# silicon carbide paper, 300~500 revs/min of polished machine revolution, along 45 degree of direction rubbing downs；Fine grinding: 1200# metallographic
Sand paper, 200~250 revs/min of polished machine revolution, along 45 degree of direction rubbing downs, removal corase grinding trace.Polishing: being 800-1200 with revolving speed
Rev/min polished machine polished.Surface roughness tester test sample surface roughness during the grinding process, and metal is disconnected
Surface wear characterization is required with surface roughness of the scanning electron microscope to sample, the partial size of Sand paper for polishing, the hardness of sample, polishing
Amplification factor of angle and scanning electron microscope etc. all influences the requirement to specimen surface roughness, and it is thick to be empirically derived calculating standard
RugosityFormula:
Wherein, A is the first impact factor, usually 1.2 × 10-4~2 × 10-4Between；θ is grinding angle, and unit is
Degree；H is the hardness of sample, N；R1、R2、R3It is followed successively by polishing for the first time, corase grinding, fine grinding sand paper partial size, unit is micron；α1、α2
For constant, α1=0.25, α2=0.35；Κ is correction factor, usually -0.43 × 10-6~-0.2 × 10-6Between；
Standard roughness is calculated according to formulaBy A=1.5 × 10-4, θ=45 °, hardness H is HRC55, R1=14 μm,
R2=10 μm, R3=5 μm, α1=0.25, α2=0.35 and Κ=- 0.33 × 10-6, obtain standard roughness
At this point, being tested to obtain R with surface roughness testera=2 μm,Sample is needed to continue to polish.
WhenWhen specimen surface roughness reach test request, carry out corrosion treatment.
Corrosion treatment: it after sample etching solution etch, is cleaned and is dried up with clear water.
Embodiment 2
A kind of preparation method of Material Wear section sample, comprising the following steps:
Pretreatment: being cleaned by ultrasonic 20 minutes with dehydrated alcohol, and acetone is cleaned by ultrasonic 10 minutes after drying, drying for standby.
Step 1: chemical nickel plating.Nickel-plating liquid is warming up to 60 DEG C, the sample handled well is placed in plating solution, has been seen whether
Bubble is emerged, and is stirred continuously plating solution.Plating 40min or more, thickness of coating reach 1.2mm；The plating piece plated is plated certainly later
It takes out, is eluted with water in liquid, dry up, nickel coating protects worn area, to guarantee that worn area becomes in subsequent processing
Shape.Wherein, the configuration proportion of nickel-plating liquid are as follows: nickel sulfate 25-35g/L, sodium hypophosphite 25-35g/L, sodium acetate 15-25g/L,
Lactic acid 15-25g/L, 5~15mL/L of propionic acid, 90~140mg/L of Potassiumiodate, 50~80mg/L of cetyl trimethylammonium bromide.
Step 2: as shown in Figure 1, by Wear specimens along perpendicular to rubbing surface, be parallel to glide direction and be cut into two parts；
As shown in Fig. 2, two parts sample is symmetrically stacked, worn area is in contact and guarantees that two sections are parallel to each other and in the same side.
Step 3: sample will be stacked and be put into embedding die, sample is fixed in mold, from embedding die sprue gate to two
Casting metal conductive copper paste in the gap of wear surface, room temperature cooling, conductive copper paste are attached fixation to sample, as shown in Figure 3
For the structure of the sample after fixation, wherein the conductive layer 104 that conductive copper paste is formed connects upper layer and lower layer nickel coating 103, by two
Sample is divided to be integrally fixed, nickel coating protects worn area 102, and wherein the depth of worn area 102, pattern propose research abrasion mechanism
For reference.
Step 4: sample carries out sand paper polishing, polishing and corrosion treatment.
Wherein, polishing, which is divided into, polishes, roughly grinds and three step of fine grinding, and the direction of polishing and casting area are in 45° angle.It polishes: using
600# silicon carbide paper, grinding angle are 45 degree, and the revolution of polished machine is set as 200~300 revs/min, and sample is made one and is put down
Face；Corase grinding: use 800# silicon carbide paper, 300~500 revs/min of polished machine revolution, along 45 degree of direction rubbing downs；Fine grinding: 1200# metallographic
Sand paper, 200~250 revs/min of polished machine revolution, along 45 degree of direction rubbing downs, removal corase grinding trace.Polishing: being 800-1200 with revolving speed
Rev/min polished machine polished.Surface roughness tester test sample surface roughness during the grinding process, and metal is disconnected
Surface wear characterization is required with surface roughness of the scanning electron microscope to sample, the partial size of Sand paper for polishing, the hardness of sample, polishing
Amplification factor of angle and scanning electron microscope etc. all influences the requirement to specimen surface roughness, and it is thick to be empirically derived calculating standard
RugosityFormula:
Wherein, A is the first impact factor, usually 1.2 × 10-4~2 × 10-4Between；θ is grinding angle, and unit is
Degree；H is the hardness of sample, N；R1、R2、R3It is followed successively by polishing for the first time, corase grinding, fine grinding sand paper partial size, unit is micron；α1、α2
For constant, α1=0.25, α2=0.35；Κ is correction factor, usually -0.43 × 10-6~-0.2 × 10-6Between；
Standard roughness is calculated according to formulaBy A=1.5 × 10-4, θ=45 °, hardness H is HRC35, α1=0.25,
α2=0.35 and Κ=- 0.7 × 10-6, obtain standard roughnessAt this point, testing to obtain with surface roughness tester
Ra=1.5, sample continues to polish.
WhenWhen specimen surface roughness reach test request, carry out corrosion treatment.
The present invention is include at least the following beneficial effects: 1, carrying out chemical nickel plating to sample worn area surface, prevent from cutting
It cuts, destroy worn area pattern during grinding and buffing.2, it is replaced inlaying resin with metal conductive fluid, solidification effect is inlayed in guarantee
While, improve measurement accuracy.3, using formula gauging surface roughness, for judging that grinding and buffing process whether can
Reach sample testing requirements, saves the time and improve sample preparation efficiency.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With.It can be applied to various suitable the field of the invention completely.It for those skilled in the art, can be easily
Realize other modification.Therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (9)
1. a kind of preparation method of Material Wear section sample, which comprises the following steps:
Step 1: nickel-plating liquid is warming up to 50~80 DEG C, sample is placed in plating solution, stirring 30~50min of plating solution, acquisition 0.5~
2mm nickel plating protective layer；
Step 2: Wear specimens along perpendicular to rubbing surface, be parallel to glide direction and be cut into two parts, two parts sample is stacked,
Worn area is in contact and guarantees that two sections are parallel to each other and in the same side；
Step 3: sample will be stacked and be put into embedding die, after fixation, the casting metal conduction slurries into the gap of two wear surfaces,
Room temperature cooling；
Step 4: sample carries out sand paper polishing, polishes and measure sample surfaces roughness Ra, and calculate the standard roughness of sample
Wherein, A is the first impact factor, 1.2 × 10-4~2 × 10-4Between value；θ is grinding angle；H is the hard of sample
Degree；R1、R2、R3It is followed successively by polishing for the first time, corase grinding, fine grinding sand paper partial size；α1、α2For constant α1=0.25, α2=0.35；K is
Correction factor, -0.43 × 10-6~-0.2 × 10-6Between value；
WhenWhen specimen surface roughness reach test request, carry out corrosion treatment.
2. the preparation method of Material Wear section sample as described in claim 1, which is characterized in that the step 1
Sample first carries out 5~10min of ultrasonic cleaning.
3. the preparation method of Material Wear section sample as described in claim 1, which is characterized in that the step 3
The surrounding of sample is fixed in embedding die.
4. the preparation method of Material Wear section sample as claimed in claim 3, which is characterized in that the embedding die
Equipped with sprue gate.
5. the preparation method of Material Wear section sample as described in claim 1, which is characterized in that the metallic conduction
Slurries are conductive silver paste or conductive copper paste.
6. the preparation method of Material Wear section sample as described in claim 1, which is characterized in that in the step 4
Polishing and polishing direction and casting area at 45 degree of angles.
7. the preparation method of Material Wear section sample as claimed in claim 6, which is characterized in that the polishing is divided into
It polishes, roughly grind and three step of fine grinding.
8. the preparation method of Material Wear section sample as claimed in claim 6, which is characterized in that the polishing, which is used, to be turned
Speed is polished for 200-1200 revs/min of polished machine.
9. the preparation method of Material Wear section sample as described in claim 1, which is characterized in that the corrosion treatment
To be cleaned and being dried up with clear water with after etching solution etch.
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| CN104181027A (en) * | 2014-08-22 | 2014-12-03 | 南京市产品质量监督检验院 | Method for preparing gold metallographic sample and displaying texture of sample |
| CN105352966A (en) * | 2015-09-29 | 2016-02-24 | 邢台钢铁有限责任公司 | High carbon steel continuous casting billet internal quality inspection method |
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Patent Citations (6)
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| CN102095624A (en) * | 2011-02-25 | 2011-06-15 | 首钢总公司 | Preparation of ultralow-carbon sheet metallographic phase sample and tissue display method |
| CN102323119A (en) * | 2011-05-25 | 2012-01-18 | 武汉钢铁(集团)公司 | Method for preparing rust layer sample for being observed by scanning electron microscope |
| CN102866048A (en) * | 2012-09-28 | 2013-01-09 | 昆明理工大学 | Preparation method of metallographic display sample of Ti-Cu laminar composite |
| CN103868775A (en) * | 2014-03-26 | 2014-06-18 | 西安热工研究院有限公司 | Metallographic sample preparation method for measuring thickness of oxide skin of boiler heating surface |
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