Metrology Programme for Nanotechnologies in CENAM …€¦ · Metrology Programme for...

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Prepared by: N. Gonzalez

Metrology Programme for Nanotechnologies in CENAM

(ProMetNano)

Norma Gonzalez, Directorate of Materials Metrology, CENAM

Awareness Seminar: Metrology in Chemistry and Nanometrology

SIM CMWG, San Jose, Costa Rica

May 19, 2016

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Topics

• Issues about measurements

• Overview of nanotechnology in Mexico

• Metrology Programme for Nanotechnologies

• Some activities in nano

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Measurement is the core of modern society

Quality of life

Fair trading

Industrial competitiveness

Workplace health and safety regulations

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World metrology day

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Nanotechnology

Nanotechnology

The application of scientific knowledge to manipulate and control matter in the nanoscale to make use of size- and structure-

dependent properties and phenomena distinct from those associated with individual atoms or molecules or with bulk materials.

(Source: ISO/TS 80004-1:2010)

Nanoscale

Size range from approximately 1 nm to 100 nm (Source: ISO/TS 80004-1:2010)

1814 consumer products from 622 companies in 32 countries

Vance, M. E., Kuiken, T.,

Vejerano, E. P.,

McGinnis, S. P.,

Hochella, M. F., Jr.,

Rejeski, D. and Hull, M.

S.

(2015) Nanotechnology

in the real world:

Redeveloping the

nanomaterial consumer

products

inventory. Beilstein

Journal of

Nanotechnology, 6, 1769-

1780.

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What’s so special about the nanoscale?

Properties of materials are size-dependent in this scale range.

…unique physical, chemical, mechanical, and optical properties of

materials that naturally occur at that scale.

Morphology Size

Silver nano-objects synthetized by A.

Manzano’s group, CINVESTAV Unidad

Queretaro. Image courtesy by FEI Company

Mexico

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Benefits and Risks

The introduction of any new material or product into commerce, there is both the potential for positive societal benefits as well as the potential risk of harm to humans or the environment during the production, use and disposal of these new products.

Due to the unique nature of nanomaterials, the current methodologies employed to conduct risk assessments, toxicological assessments and life cycle analysis of products containing nanomaterials may be ineffective or may not currently exist.

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Characterization and regulatory gaps of nano-products

• No agreed protocols for physico-chemical characterization

• Existing ‘test methods’ may not be suitable for nanoscale devices and dimensions

• Measurement techniques and instruments need to be developed and/or standardized

• Calibration procedures and CRMs needed for measurement instruments at nanoscale

Therefore, on

the basis of the study by

Heinrich et al. [1995] and the

pattern of pulmonary

inflammatory

responses, NIOSH has

determined that exposure to

ultrafine TiO2 should be

considered a potential

occupational carcinogen.

Photothermal therapy of Lewis lung

carcinoma in mice using gold nanoshells on

carboxylated polystyrene spheres

Comex battles Mexican graffiti with nanocoating technology: nano coatings are helping to keep Mexico's infrastructure graffitti-free

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Nanotechnology value chain

Basic scientific research

Applied research

New products

PRE-COMMERCIAL STAGE COMMERCIAL STAGE

Product and process

development

Experimental technological development

Reliable measurements

DISPOSAL

Environmental, health and safety; Regulation, education and ethics

Se tomó como base la ref. González J., Red de Innovación en Nanotecnología en Nuevo León (2014). Cátedra en la Facultad

de Química de la Universidad Autónoma de Querétaro

EDGE OF

KNOWLEDGE

APPLIED

KNOWLEDGE

PRODUCT –

PROCESS

PROTOTYPE

INDUSTRIAL

UPGRADING

COMERCIAL

APPLICATION

MARKET

Nanomaterials Nanointermediates Nano-enable products

Nanotechnology may become

a new non-tariff barrier

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Overview of Nanotechnology in Mexico

Industry

Government

Education and

Research

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Higher education institutions and R+D Resources

58 Institutes

159 Laboratories

17 Pilot plants

4 Networks

Záyago-Lau, E.; Foladori, G., Economía, Sociedad y Territorio, Vol. X, Núm.

32, enero-abril, 2010, pp. 143-178

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Education and Research Capabilities

1. CINVESTAV México

2. CINVESTAV Mérida

3. CINVESTAV Querétaro

4. CINVESTAV Saltillo

5. CIITEC -IPN

6. ESFM -IPN

7. IF- UNAM

8. IQ- UNAM

9. CIE- UNAM

10. IIM-UNAM

11. CFATA-UNAM

12. CCADET- UNAM

13. FC- UNAM

14. CCMC- UNAM

15. IMP

16. ININ

17. CENAM

18. CIMAV

19. CIQA

20. CIDESI

21. CIATEC

22. CICY

23. CICESE

24. CIAD

25. CIATEJ

26. CIBNOR

27. CIDETEQ

28. CIO

29. CIATEQ, A.C.

30. COMIMSA

31. IPICYT

32. BUAP

33. UACH

34. UACJ

35. UANL

36. UASLP

37. UADY

38. UAEH

39. UAM-Azcapotzalco

40. UAM-Iztapalapa

41. UDG

42. UG

43. UNISON

44. UMSNH

45. UV/MICRONA

46. ITC

47. ITS

48. ITH

49. ITQ

50. UDEM

51. UDLA

52. UAMS

53. UTM

54. UPChiapas

55. UAZ

56. ITZ

6-IPN 8 - UNAM

3- Research

Institutions

“Sectorizadas”

14- CPI (PRC),

CONACYT System 25- IES (HEI) 56 Institutions

1

2 3

4

5 6 7

8 9

14

12 13

11

10 15

16

17

18

19

20 21

22

23

24

25

26

27 28 29

30

31

32

33

34

35

36

37 38

39 40

41

42

43

46

45 44

47

48

49

50

51 52 53

54

55

56

34 with more than 10 PhDs

Source: 2008

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13

4

75

14

28

12

8

1

7

8

1

1

4

2

Innovation Projects related with Nanotechnology

CONACYT Fund for Innovation (2009-2012)

17

1

1

INNOVATION FUND (2009-2011) (COMPANIES)

AREA PERCENTAGE

Nanofillers(polymers 75%) 33%

Nanomedicine/ Nanobiotechnology 16%

Nanostructured coatings 11%

Paper 6%

Others 35%

51 awarded USD 225 000/per project

State Projects Approved

Nuevo León 75 28

Edo. Mex. 28 5

Distrito Federal 17 5

Coahuila 14 5

Guanajuato 12 3

Sonora 8 2

San Luis Potosí 8 2

Querétaro 7 4

Chihuahua 4 1

Jalisco 4 1

Sinaloa 2 0 Baja California

Sur 1 0

Baja California 1 0

Colima 1 0

Hidalgo 1 0

Michoacán 1 0

TOTAL 177 58 Source: Dir. Tec. CONACYT

549 PhD in Mexico 6 % of publications

> 4000/10 years

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Nanoscience and Nanotechnology Network (CONACYT)

1. CIMAV

2. CIQA

3. CIDESI

4. CIATEC

5. CICY

6. CICESE

7. CIAD

8. CIATEJ

9. CIDETEQ

10. CIBNOR

11. CIO

12. CIATEQ, A.C.

13.COMIMSA

14. CINVESTAV México

15. CINVESTAV Querétaro

16. CINVESTAV Saltillo

17. CIITEC del IPN

18. ESFM del IPN

19. IIM de la UNAM

20. IF de la UNAM

21. BUAP

22. UACH

23. UACJ

24. UANL

25.UASLP

26.UADY

27. UAEH

28. UAM-

Azcapotzalco

29. UAM-Iztapalapa

30. UdeG

31. UG

32. UNISON

33. UMSNH

34. UV/MICRONA

35. CENAM

36. IPICYT

37. ITC

38. ITS

39. ITZ

Key Area Leaders Key Competency Areas

Process and equipment design

Nanometrology

Bionanotechnology

Computational Simulation

Polymeric Nanostructures

Inorganic Nanostructures

Nanoparticles

CIDESI

CENAM

CIAD

CINVESTAV

CIQA

CIITEC-IPN

CIMAV

Participation

≈350 Scientists

Source: J. González H., 2010

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n-Industrial Activities

GEOGRAPHIC LOCATION

101 COMPANIES using NANOTECHNOLOGY in 2013

NL

PRODIAT Program for high technology industry

development, nanotechnology,

biotechnology and ICTs

39 %

31 % 10 %

4 % 3 %

2 %

3 %

Foladori et al., 2013

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Nanotechnology Cluster in Nuevo Leon

3 DEVELOPMENT DIRECTIVES

Start Ups

Micro- clustering

20 microcluster with 50 PYMES

Projects with and betwwen

Cluster Companies

Capital

Privado

35 ACTIVE MEMBERS

Source: J. González H., UAQ, 2014

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Nanotech Incubator

Ad

ded

Va

lue

( $

/ k

g )

Re

gis

tred

pa

ten

ts 7

0%

25

% 5

%

Semiconductores

Apparatus Liquid

Crystals

Fiber

Optics

Pharmaceutical

Compositions

Thin

Films

Laser

Beams

Substrates

Semiconducters

Dielectric

Products/Market

High Technology

Products/Market

Medium-high Technology

Products/Market

Medium-Low Technology

Optical

Systems

Nucleic

Acids

Displays

Imaging

Systems

Sources

of Light

Dielectric

Metallic

Óxides

Aqua's

Solutions

Catalysis

Resins

Compositions

Dielectric

Materials

Refractive

Indexes Fibers

Textiles

Water – Air

Purification

Materials

Cement

Materials

Glass

Packaging

Polymers

Steel

Elastomers

Thermoplastics

Food

Products

Personal

Healthcare

Inhibiters

Protease

Water

Treatment

Biotechnology

Scientific/Technological Complexity

Oportunidades para México

Pla

tfo

rms

De

fin

itio

n

for

Na

no

In

cu

ba

tor

in N

L

Value Map of Nanotech Products

Launched / September 2009

CIMAV: Technical Administration

Functions: Start-up and support to existing

companies


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Scaled Products from Incubator

UV protection film for agroindustrial use

Bactericide + fungicide Mechanical strength + UV

Low friction coefficient lubricant Hydrophobic and oleophobic properties

v

Nanotech Cluster Members

Mechanical properties improved foam


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Stakeholders for standards and regulations

ISO TC 229 Nanotechnology

OECD- Working Party on

Manufactured Nanomaterials

(WPMN)

Consultative Committee for

Amount of Substance – Metrology in

Chemistry

BIPM

VAMAS

National Technical Committee of

Standardization in Nanotechnology and International Standardization

Committee Mirror of ISO TC 229

INDUSTRY EDUCATION AND

RESEARCH GOVERNMENT

Initiative for Nanotechnology development in

Mexico,

Nanoscience and

Nanotechnology Network,

CONACYT

European Commission Projects

Horizon 2020:

BISNANO, NANOSAFETY

United States-Mexico High-Level

Regulatory Cooperation Council

(Nanotechnology)

•Guidelines on regulations for

nanotechnologies to foster

competitiveness and protect the

environment, the human health and the safety of the

consumers

Regulation Bodies:

SE

STPS

COFEPRIS

SAGARPA

SEMARNAT

INECC Competitiveness, strengthening of economy, health and environment

protection

8 published voluntary

Mexican standards

and 8 in preparation

VAMAS TWA-2,

TWA-33, TWA-34

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The National Metrology Institute in Mexico

Staff: 295 people ≈ 155 Technical

activities

4 Technical Areas

731 CMC in

BIPM-KCDB

150 international

comparisons

> 60 on-site peer

reviews

>3000 calibrations/yr

> 300 CRM

> 44 National PT/yr

and other services

Formal activities

since 1994

68 National

Standards

Electrical Physical Materials Mechanical

Electromagnetic measurement

Thermometry

Time and frequency

Radiofrequency

Acoustic and vibrations

Optics and radiometry

Reference materials

Inorganic analysis

Organic analysis

Flow and volume

Force and pressure

Mass and density

Dimensional

Technology

Services

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Mission Support different sectors of society in order to satisfy present and future metrological needs, establishing national measurement standards, developing reference materials and disseminating its accuracy, through technological services of the highest quality, aiming to increase the country’s competitiveness, contribute to sustainable growth and improve the quality of life of citizens.

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The Need for Standards and Metrology

• Nanoscience can only evolve into nanotechnology once the measurement problems and metrology are under control

• Economic impacts from product development and commercialization demand standards

• Workplace safety, environment and health are the key drivers during this transition

• The role of NMIs

• Traceable instrumentation and measurement techniques for calibration

• Development and calibration of artefact standards and reference materials

• Suitable models for uncertainty evaluation

• Conducting international measurement comparisons of independently realized quantities

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Broadening measurement capabilities

SI

m

kg

A

mol s

K

cd

N y N

Size

Metrology Programme

for Nanotechnologies

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ProMetNano Improvement or development of new equipment / measurement devices

Improvement or development of new measurement standards and methods

Support to improve or develop new process

HEI

Industry

Government

Measurements are essential to all stages of materials and product life cycles

Novel measurements capable of probing nanoscale dimensions and nanoscale entities

• Biotechnology

• Climate change

• Energy

• Automotive

• Health

• Safety

• Food

• Aerospace

• Others…

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CENAM Nanometrology – Key areas

Linking the nanometre to the metre

Provide traceability for nanoscale dimensional

measurements using a Metrological Atomic

Force Microscope (m-AFM)

Metrology for nanomaterials

Nanoparticle characterisation

Evaluation of instrumentation

Instrument and method development

Reference materials Narayan Poudyal and J Ping

Liu 2013 J. Phys. D: Appl. Phys.

46 043001

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Traceable dimensional nano measurement

SI m

Iodine-stabilized laser

Calibration of m-AFM interferometry laser

m-AFM

Commercial AFM

Calibration artefacts

Measurement nanoparticles

Unit realization

International agreement

(CGPM /BIPM)

Accredited or final

user’s lab

In-field or lab

calibration

Linking the nanometre to the metre

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Metrology for nanomaterials

Properties cannot be extrapolated from the macro scale.

Enormous variety of nanomaterials and characterization techniques.

Physico‐chemical metrology is still in understanding process.

No consensus about which properties are the crucial ones for both beneficial and detrimental effects.

The interaction of nanomaterials with the environment is crucial but poorly understood.

No routine methods are available for analysing nanomaterials in matrices (metal, ceramics, polymers, …)

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Size measurement

¿What is the right particle diameter?

DLS TEM SEM AFM

8.5 nm ± 0.3 nm 8.9 nm ± 0.1 nm 9.9 nm ± 0.1 nm 13.5 nm ± 0.1 nm

np-Au

Nominal diameter: 10 nm NIST Report of Investigation, RM 8011, 2007

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what is the measurand? which unit?

Identifying and counting particles in air

Identifying and counting their

metabolites in biological matrices

(¿?)

• Measuring their functional properties

(¿?)

But, particles unstable and reactive

• Undergo transformation

Nanoparticle measurements questions

Symmetric objects Morphology

parameters but others…

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Size measurement

• Different physical principles, e.g., • SEM, TEM: electron scattering/diffraction– direct

method • DLS: Brownian motion in a liquid – ‘hydrodynamic’

diameter • AFM: force measurement

• Each type of measurement needs different sample preparation

• Measured ‘size’ is defined differently

• Use of multiple techniques

• Relevance for toxicity testing?

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np-Ag – candidate of reference material

• Why

• One of the most used nanomaterial for manufacturing products,

• One of the most used for research institutions,

• Research and industry labs are interested on it to evaluate electron microscopes and DLS performance and for risk assessment protocols,

• Regulation support,

• Foster synergic collaboration between industry-CENAM-government-HEI.

• Intended uses

• Develop and evaluate in vitro and in vivo assays designed to assess the biological response,

• Evaluate and qualify methodology and instrument performance related to the physical and dimensional characterization of nanoscale particles,

• Facilitate interlaboratory comparisons and benchmarking,

• Develop and evaluate assays to assess the impact of nps in the environment and the risks to human health and safety.

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Nanomaterial candidate

• Mexican company

• Biological process

npAg

TEM 15 nm ± 5.3 nm

DLS 55 nm

UV-VIS

424 nm

Potencial zeta

11.9 mV ± 4.4 mV

APCI-

MS

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Process of RM proposed

Nano-objetos de plata sintetizados por el CINVESTAV-Qro, imagen cortesía de Zeiss

Imagen obtenida por TEM de nanopartículas de plata proporcionadas por Lotto-Labs, cortesía CNMyN-IPN.

Development of

measurement

method and

instrumentation

Method

reproducibility Validation of

method

Test material Reference

material

Certified

reference

material

Production

procedure

Homogeneity

and stability

studies

Certified

assigned value

• What is particle aspect?

– Size

– Morphology

• What is the particle composition?

– Composition of all volume

– Surface composition

– Impurities

• How interact with environment?

– Surface charge

– Aggregation / agglomeration state

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Final thoughts

Metrology at the nanoscale is critical for the development of nanotechnology,

both for scientific understanding and for viable commercial activities.

No single technique will be able to provide all of the critical metrology for

nanoscale systems.

Ongoing challenges include the development of instrumentation with a level of

complexity for use by scientists and in the development of physical

understanding of the response from complex heterogeneous nanometer-scale

systems.

• Useful to consider gateway projects to establish traceability at the nanoscale

• certified reference materials

• instrumentation with embedded traceability

• Many challenges exist

• types of instruments produce different results

• morphology of nanomaterials/nanoparticles influences measurements

• sample preparation is critical

• …

• Cooperation and collaboration between NMIs is the most productive path

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Next steps...

• Consolidate CENAM infrastructure – Laboratories, equipments, human resources.

• Development of Nanometrology Projects in collaboration with RDI institutions, regulatory agencies and industry.

• Strengthening of Standards, Metrology and Conformity Assessment System in Mexico.

• Continue International collaboration.

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Thank you for your attention

Norma González

Centro Nacional de Metrología

MÉXICO

Phone: +52(442) 211 0500

e-mail: [email protected]

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